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HRID1486088

反应详情

EQUATION

反应方程式

HRID 1486088 的结构方程式

REACTANTS

反应物

2
结构：[Na+].[OH-]
HCID14798

Sodium Hydroxide

HNaO

结构：CC(=O)N1C(=O)[C@@H](NC(=O)OC(C)(C)C)[C@H](C)N(C(C)=O)c2cc(C#N)ccc21
HCID131736780

未命名化合物

PRODUCTS

生成物

1
结构：CC(=O)N1c2cc(C#N)ccc2NC(=O)[C@@H](NC(=O)OC(C)(C)C)[C@@H]1C
HCID131736779

未命名化合物

收率 39%

AUXILIARIES

试剂、催化剂与溶剂

2
结构：CO
溶剂HCID887

Methanol

CH4O

结构：CCOC(C)=O
溶剂HCID8857

Ethyl acetate

C4H8O2

PROCEDURE

实验过程

To a rt solution of tert-butyl(3S,4S)-1,5-diacetyl-7-cyano-4-methyl-2-oxo-2,3,4,5-tetrahydro-1H-benzo[b][1,4]diazepin-3-ylcarbamate (413 mg, 1.03 mmol) in MeOH (10.3 ml) was added 1 M aq. sodium hydroxide (1.13 ml, 1.13 mmol), dropwise. The reaction was stirred for 30 min, then diluted with EtOAc, washed with H2O and sat. aq. NaCl, dried over Na2SO4, filtered, and concentrated. The crude material was purified by flash chromatography to provide tert-butyl(2S,3S)-1-acetyl-8-cyano-2-methyl-4-oxo-2,3,4,5-tetrahydro-1H-benzo[b][1,4]diazepin-3-ylcarbamate (144 mg, 39%) as a white solid. MS m/z 381 (MNa)+.

WORKUP

后处理

  1. washwashed with H2O and sat. aq. NaCl
  2. dry with materialdried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe crude material was purified by flash chromatography