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Sodium hydrosulfide → Methyl 4-mercapto-2-methyl-5-nitrobenzoate

HRID 1942491
ノート
印刷プレビュー

反応式

HRID 1942491 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.[SH-:16].[Na+]>CO>[SH:16][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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 28015Sodium hydrosulfideHCID 10633188Methyl 4-chloro-2-methyl-5-nitrobenzoate

生成物 1

HCID 58376194Methyl 4-mercapto-2-methyl-5-nitrobenzoate収率 97.7%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of methyl 4-chloro-2-methyl-5-nitrobenzoate (1.21 g) in methanol (20 ml) was added sodium hydrosulfide (561 mg), and the mixture was refluxed with stirring for 2 hours. After the reaction was complete, the reaction solution was concentrated, and methanol was concentrated under reduced pressure. Then, to the resultant were added water and 2N hydrochloric acid, and the mixture was extracted with ethyl acetate. The organic layer was dried over sodium sulfate, filtered, concentrated under reduced pressure. The obtained residue was purified by column chromatography to give the title compound (1.17 g).

後処理

  1. temperaturethe mixture was refluxed
  2. concentrationthe reaction solution was concentrated
  3. concentrationmethanol was concentrated under reduced pressure
  4. additionThen, to the resultant were added water and 2N hydrochloric acid
  5. extractionthe mixture was extracted with ethyl acetate
  6. dry with materialThe organic layer was dried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. customThe obtained residue was purified by column chromatography

出典と根拠

ORDレコード
ord-4e30d340965041deb32d163a4d305239
出典データセット
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08389511B2

反応ノート

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