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HRID1505571

反应详情

EQUATION

反应方程式

HRID 1505571 的结构方程式

REACTANTS

反应物

3
结构：CC(C)CN
HCID6558

Isobutylamine

C4H11N

结构：O=C([O-])[O-].[Na+].[Na+]
HCID10340

Carbonic acid sodium salt (1:2)

CNa2O3

结构：CC(C)(C)OC(=O)N[C@@H](Cc1ccccc1)[C@H](O)CCl
HCID7146645

tert-Butyl [(2S,3S)-4-chloro-3-hydroxy-1-phenylbutan-2-yl]carbamate

C15H22ClNO3

PRODUCTS

生成物

1
结构：CC(C)CNC[C@@H](O)[C@H](Cc1ccccc1)NC(=O)OC(C)(C)C
HCID9902339

tert-Butyl {(2S,3R)-3-hydroxy-4-[(2-methylpropyl)amino]-1-phenylbutan-2-yl}carbamate

C19H32N2O3

收率 93.6%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：O
溶剂HCID962

Water

H2O

2 次

CONDITIONS

反应条件

温度
62.5 °C

PROCEDURE

实验过程

The mixture of [(1S,2S)-3-chloro-2-hydroxy-1-(phenylmethyl)propyl]carbamic acid tert-butyl ester (5, 100 g), isobutyl amine (294 g), sodium carbonate (31.3 g) and water was heated to 60-65° C. and maintained for 3 hours. After completion of reaction water (200 mL) was added and distilled out excess isobutyl amine under vacuum at below 75° C. Water (800 mL) was added to the distillate, cooled to 25-35° C. and stirred for 2 hours. The obtained solid was filtered and washed with water to get title compound 4 (yield 105 g).

WORKUP

后处理

  1. temperaturemaintained for 3 hours
  2. additionwas added
  3. distillationdistilled out excess isobutyl amine under vacuum at below 75° C
  4. additionWater (800 mL) was added to the distillate
  5. temperaturecooled to 25-35° C.
  6. filtrationThe obtained solid was filtered
  7. washwashed with water