Sodium Chloride → Methyl 4-[(2-ethoxy-1-methyl-2-oxoethyl)thio]-2-methyl-5-nitrobenzoate

HRID 1942494ノート

反応式

HRID 1942494 の反応式
Cl[C:2]1[C:11]([N+:12]([O-:14])=[O:13])=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[C:4]([CH3:15])[CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[SH:22][CH:23]([CH3:29])[C:24]([O:26][CH2:27][CH3:28])=[O:25].[Cl-].[Na+]>CN(C)C=O>[CH2:27]([O:26][C:24](=[O:25])[CH:23]([S:22][C:2]1[C:11]([N+:12]([O-:14])=[O:13])=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[C:4]([CH3:15])[CH:3]=1)[CH3:29])[CH3:28]

参加物

6

反応物 4

HCID 5234Sodium ChlorideHCID 11430Potassium CarbonateHCID 519709Ethyl 2-mercaptopropionateHCID 10633188Methyl 4-chloro-2-methyl-5-nitrobenzoate

生成物 1

HCID 67333305Methyl 4-[(2-ethoxy-1-methyl-2-oxoethyl)thio]-2-methyl-5-nitrobenzoate収率 111.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

To a solution of methyl 4-chloro-2-methyl-5-nitrobenzoate (2.52 g) in N,N-dimethylformamide (20 ml) were added potassium carbonate (3.04 g) and ethyl 2-mercaptopropionate (2.2 g), and the mixture was stirred at 80° C. for 4 hours. After the reaction was complete, to the mixture was added a saturated aqueous sodium chloride solution, and the mixture was extracted with ethyl acetate. The organic layer was dried over sodium sulfate, filtered, concentrated under reduced pressure to give methyl 4-[(2-ethoxy-1-methyl-2-oxoethyl)thio]-2-methyl-5-nitrobenzoate (4.0 g). Subsequently, the title compound was obtained in a similar manner to Reference Example 2.

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. dry with materialThe organic layer was dried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-e70aba7b41eb46e3be9735aa1df62a99
出典データセット
uspto-grants-2013_03
特許番号
US08389511B2

反応ノート

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