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HRID2353858

反应详情

EQUATION

反应方程式

HRID 2353858 的结构方程式

REACTANTS

反应物

2
结构：CCOC(=O)CCCN(c1ccccc1C(=O)OC)S(=O)(=O)c1ccc(C)cc1
HCID266879

Methyl 2-[(4-ethoxy-4-oxobutyl)(4-methylbenzene-1-sulfonyl)amino]benzoate

C21H25NO6S

结构：CC(C)(C)[O-].[K+]
HCID23665647

2-Methyl-2-propanol, potassium salt

C4H9KO

PRODUCTS

生成物

1
结构：CCOC(=O)C1CCN(S(=O)(=O)c2ccc(C)cc2)c2ccccc2C1=O
HCID12435934

Ethyl 1-(4-methylbenzene-1-sulfonyl)-5-oxo-2,3,4,5-tetrahydro-1H-1-benzazepine-4-carboxylate

C20H21NO5S

收率 64.9%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：Cc1ccccc1
溶剂HCID1140

Toluene

C7H8

PROCEDURE

实验过程

To a heated mixture of potassium t-butoxide (371 g, 3.58 mol) in toluene (4 l) at 70° C. was added 2-[(3-Ethoxycarbonyl-propyl)-(toluene-4-sulfonyl)-amino]-benzoic acid methyl ester (750 g, 1.79 mol). After the addition was completed, the mixture was cooled to room temperature then poured into ice water. The extraction with CH2Cl2 was successively done, and organic layer was dried over MgSO4 and concentrated under reduced pressure to afford crude compound 5-Oxo-1-(toluene-4-sulfonyl)-2,3,4,5-tetrahydro-1H-benzo[b]azepine-4-carboxylic acid ethyl ester (450 g) as a mixture of Me and Et esters.

WORKUP

后处理

  1. additionAfter the addition
  2. extractionThe extraction with CH2Cl2
  3. dry with materialorganic layer was dried over MgSO4
  4. concentrationconcentrated under reduced pressure