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Methanethiol → HCID 3642305、化合物

HRID 1733649
ノート
印刷プレビュー

反応式

HRID 1733649 の反応式
CS[C:3]([C:9]1[CH:14]=[CH:13][C:12]([C:15]([C:17]2[S:18][CH:19]=[CH:20][CH:21]=2)=[O:16])=[CH:11][CH:10]=1)([CH3:8])[C:4]([O:6][CH3:7])=[O:5].[Na].CS.[Cl-].[NH4+]>CO>[S:18]1[CH:19]=[CH:20][CH:21]=[C:17]1[C:15]([C:12]1[CH:13]=[CH:14][C:9]([CH:3]([CH3:8])[C:4]([O:6][CH3:7])=[O:5])=[CH:10][CH:11]=1)=[O:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 878MethanethiolHCID 25517Ammonium ChlorideHCID 5360545SodiumHCID 12917659HCID 12917659、化合物

生成物 1

HCID 3642305HCID 3642305、化合物収率 47.5%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

Methyl α-methylthio-α-[p-(2-thienylcarbonyl)-phenyl]propionate (288 mg) was dissolved in 1 ml of anhydrous methanol, and 1.0 ml of a methanol solution (2.34 M) of sodium salt of methyl mercaptan was added. The mixture was stirred at room temperature for 1 hour and heated under reflux for 30 minutes. After cooling, an aqueous solution of ammonium chloride (1.5 g/20 ml) was added to the reaction mixture. The mixture was extracted with 20 ml of methylene chloride and twice with 10 ml of methylene chloride. The extract was washed with 20 ml of a saturated aqueous solution of sodium hydrogen carbonate and with 10 ml of water, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to afford 117 mg of methyl α-[p-(2-thienylcarbonyl)phenyl]propionate in a yield of 47%.

後処理

  1. temperatureheated
  2. temperatureunder reflux for 30 minutes
  3. temperatureAfter cooling
  4. extractionThe mixture was extracted with 20 ml of methylene chloride and twice with 10 ml of methylene chloride
  5. washThe extract was washed with 20 ml of a saturated aqueous solution of sodium hydrogen carbonate and with 10 ml of water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-68a9fabe328349fc8cdb451347ba69de
出典データセット
uspto-grants-1980_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04242519

反応ノート

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