反应 #4117986
相关文献 (1)
openreactiondata ↗doi:10.1039/C8SC04228D
反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-f65dc90922f346da98345089edcbc640暂无可渲染的结构数据
CCOC(=O)C1CCCC1N产品信息
2-氨基环戊烷甲酸乙酯(CAS 38052-23-2)的产品身份、结构标识及相关反应资料,供化学中间体检索、研发和采购评估使用。
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合成路线数据
7 条反应 · 7 篇文献
反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-f65dc90922f346da98345089edcbc640反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-3f43d9139fa0463cb15aee0103d6f901反应条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 4.8 g of diketene were added to a mixture of 9 g of 1-amino-2-carbethoxy-cyclopentane and 90 ml of benzene and after stirring for 72 hours at 20° C., the mixture was evaporated to dryness under reduced pressure. The residue was chromatographed over silica gel and was eluted with an 8-2 methylene chloride-acetone mixture to obtain 7.7 g of N-(2-carbethoxycyclopentyl)-acetylacetamide with a refractive index of ND22 =1.487. 6.3 g of the latter product and 0.25 g of p-toluene sulfonic acid were added to a mixture of 4.2 g of methyl orthoformate and 60 ml of methanol and after stirring the mixture at 20° C. for 16 hours, the mixture was evaporated to dryness under reduced pressure. The residue was added to toluene and 0.5 ml of quinoline and the mixture was heated at 145° C. for 1 hour while distilling a toluene-methanol azeotrope. The mixture was evaporated to dryness under reduced pressure and the residue was chromatographed over silica gel. Elution with a 9-1 methylene chloride-acetone mixture gave 1.8 g of N-(2'-carbethoxycyclopentyl)-3-methoxy-crotonamide melting at 74° C. The RMN spectra showed it to be the E isomer. the mixture was evaporated to dryness under reduced pressure The residue was chromatographed over silica gel was eluted with an 8-2 methylene chloride-acetone mixture
来源 ID: ord-7334f064af04473db1382b5771f01fa8反应条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 4.8 g of diketene were added to a mixture of 9 g of 1-amino-2-carbethoxy-cyclopentane and 90 ml of benzene and after stirring for 72 hours at 20° C., the mixture was evaporated to dryness under reduced pressure. The residue was chromatographed over silica gel and was eluted with an 8-2 methylene chloride-acetone mixture to obtain 7.7 g of N-(2-carbethoxycyclopentyl)-acetylacetamide with a refractive index of ND22 =1.487. 6.3 g of the latter product and 0.25 g of p-toluene sulfonic acid were added to a mixture of 4.2 g of methyl orthoformate and 60 ml of methanol and after stirring the mixture at 20° C. for 16 hours, the mixture was evaporated to dryness under reduced pressure. The residue was added to toluene and 0.5 ml of quinoline and the mixture was heated at 145° C. for 1 hour while distilling a toluene-methanol azeotrope. The mixture was evaporated to dryness under reduced pressure and the residue was chromatographed over silica gel. Elution with a 9-1 methylene chloride-acetone mixture gave 1.8 g of N-(2'-carbethoxycyclopentyl)-3-methoxy-crotonamide melting at 74° C. The RMN spectra showed it to be the E isomer. the mixture was evaporated to dryness under reduced pressure The residue was chromatographed over silica gel was eluted with an 8-2 methylene chloride-acetone mixture
来源 ID: ord-7334f064af04473db1382b5771f01fa8反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-f65dc90922f346da98345089edcbc640反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-3f43d9139fa0463cb15aee0103d6f901反应条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 4.8 g of diketene were added to a mixture of 9 g of 1-amino-2-carbethoxy-cyclopentane and 90 ml of benzene and after stirring for 72 hours at 20° C., the mixture was evaporated to dryness under reduced pressure. The residue was chromatographed over silica gel and was eluted with an 8-2 methylene chloride-acetone mixture to obtain 7.7 g of N-(2-carbethoxycyclopentyl)-acetylacetamide with a refractive index of ND22 =1.487. 6.3 g of the latter product and 0.25 g of p-toluene sulfonic acid were added to a mixture of 4.2 g of methyl orthoformate and 60 ml of methanol and after stirring the mixture at 20° C. for 16 hours, the mixture was evaporated to dryness under reduced pressure. The residue was added to toluene and 0.5 ml of quinoline and the mixture was heated at 145° C. for 1 hour while distilling a toluene-methanol azeotrope. The mixture was evaporated to dryness under reduced pressure and the residue was chromatographed over silica gel. Elution with a 9-1 methylene chloride-acetone mixture gave 1.8 g of N-(2'-carbethoxycyclopentyl)-3-methoxy-crotonamide melting at 74° C. The RMN spectra showed it to be the E isomer. the mixture was evaporated to dryness under reduced pressure The residue was chromatographed over silica gel was eluted with an 8-2 methylene chloride-acetone mixture
来源 ID: ord-7334f064af04473db1382b5771f01fa8PubChem References
以下资料来自该化合物的公开数据库参考记录。
