huagongshe.com
HRID129426

反应详情

EQUATION

反应方程式

HRID 129426 的结构方程式

REACTANTS

反应物

4
结构：O=C(O)[C@H](O)[C@@H](O)C(=O)O
HCID444305

L-Tartaric acid

C4H6O6

结构：c1ccc(CN2C[C@@H]3CCCN[C@@H]3C2)cc1
HCID10198297

(4aS,7aS)-Octahydro-6-(phenylmethyl)-1H-pyrrolo[3,4-b]pyridine

C14H20N2

结构：O=C(O)[C@H](O)[C@@H](O)C(=O)O.c1ccc(CN2C[C@@H]3CCCN[C@@H]3C2)cc1
HCID10981401

未命名化合物

结构：O=C(O)[C@H](O)[C@@H](O)C(=O)O.c1ccc(CN2C[C@H]3CCCN[C@H]3C2)cc1
HCID68615090

未命名化合物

PRODUCTS

生成物

2
结构：O=C(O)[C@@H](O)[C@H](O)C(=O)O
HCID439655

未命名化合物

结构：O=C(O)[C@@H](O)[C@H](O)C(=O)O.c1ccc(CN2C[C@@H]3CCCN[C@@H]3C2)cc1
HCID22857294

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CN(C)C=O
溶剂HCID6228

N,N-Dimethylformamide

C3H7NO

2 次

CONDITIONS

反应条件

温度
18 °C

PROCEDURE

实验过程

73.6 g (0.34 mol) of cis-8-benzyl-2,8-diazabicyclo[4.3.0]nonane dissolved in 111 ml of dimethylformamide is added a drop at a time to a solution of 102.9 g (0.685 mol) of L(+)-tartaric acid in 343 ml of dimethylformamide. The batch is seeded with [R,R]-8-benzyl-2,8-diazabicyclo[4.3.0]nonane L-tartrate and gradually cooled to an interior temperature of 18° C. The crystals are suctioned off and the filtrate seeded with [S,S]-8-benzyl-2,8-diazabicyclo[4.3.0]-nonane L-tartrate and agitated until it crystallizes completely. ([S,S]-8-benzyl-2,8-diazabicyclo[4.3.0]nonane D-tartrate can be obtained from the mother liquor subsequent to concentration and release of the base by purification with D(-)-tartaric acid as described for Method I.) The product is suctioned off, washed with dimethylformamide and isopropyl alcohol, and dried in the air. The crystals are recrystallized from 88% ethanol. 52 g of [S,S]-8-benzyl-2,8-diazabicyclo[4.3-O]nonane L-tartrate trihydrate are obtained.

WORKUP

后处理

  1. customcrystallizes completely