γ-丁内酯 → 3-(Aminomethyl)-3-methyl-2,3,4,6,7,8-hexahydropyrrolo[1,2-a]pyrimidine

HRID 1151

反应方程式

HRID 1151 反应方程式
[C:1]1(=O)O[CH2:4][CH2:3][CH2:2]1.[Cl-].[NH4+].[NH2:9][CH2:10][C:11]([CH2:15][NH2:16])([CH2:13][NH2:14])[CH3:12]>O>[NH2:9][CH2:10][C:11]1([CH3:12])[CH2:15][N:16]2[CH2:4][CH2:3][CH2:2][C:1]2=[N:14][CH2:13]1

参与物

5

反应物 3

HCID 7302γ-丁内酯HCID 25517氯化铵HCID 45265302-(氨甲基)-2-甲基-1,3-丙二胺

产物 1

HCID 184074873-(Aminomethyl)-3-methyl-2,3,4,6,7,8-hexahydropyrrolo[1,2-a]pyrimidine

试剂、催化剂与溶剂 1

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

反应条件

温度
250 °C

实验过程

A mixture of 21.03 g (0.24 mol) of γ-butyrolactone and 1.31 g (24 mmol) of ammonium chloride in 114.5 g (0.98 mol) of 1,1,1-tris(aminomethyl)ethane was heated at 250° C. in an autoclave. After 1.5 h, the mixture was cooled and the excess amine and the water formed were removed by distillation. The residue was distilled at 200°-240° C./18 mbar. The yield was 22.0 g (54%) of yellowish oil. The boiling point was 117°-120° C./1 mbar. Other data concerning the product was:

后处理

  1. temperaturethe mixture was cooled

来源与证据

ORD记录
ord-58e35fa5d3104b07bb1cd637b9c2a80b
来源数据集
uspto-grants-1998_03
专利号
US05723605

关联笔记

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