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Potassium Carbonate → HCID 14528680、化合物

HRID 223720
ノート
印刷プレビュー

反応式

HRID 223720 の反応式
[SH:1][C:2]1[CH:3]=[C:4]([CH:8]([CH3:12])[C:9]([OH:11])=[O:10])[CH:5]=[CH:6][CH:7]=1.[C:13](=[O:16])([O-])[O-:14].[K+].[K+]>CN(C)C=O>[C:13]([CH:3]1[CH2:2][CH2:7][CH2:6][CH2:5][CH:4]1[CH2:8][S:1][C:2]1[CH:3]=[C:4]([CH:8]([CH3:12])[C:9]([OH:11])=[O:10])[CH:5]=[CH:6][CH:7]=1)([OH:14])=[O:16]
参加物反応条件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 11430Potassium CarbonateHCID 14528677HCID 14528677、化合物

生成物 1

HCID 14528680HCID 14528680、化合物収率 192.6%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
170 °C

実験手順

To 2-(3-mercaptophenyl)propionic acid (2.7 g) were added cis-2-(hydroxymethyl)cyclohexanecarboxylic acid lactone (2.5 g), potassium carbonate (2.5 g) and dimethylformamide (25 ml). The mixture was heated with stirring for 3 hours in an oil bath maintained at 170° C. and evaporated to dryness under reduced pressure. The residue was dissolved in water, acidified with hydrochloric acid and extracted with ethyl acetate. The ethyl acetate layers were washed with water, dried over anhydrous sodium sulfate and evaporated to dryness under reduced pressure to give the title compound (4.6 g) as an oil. IR νmaxfilm cm-1 : 1700 (C=O). MS m/e: 322 (M+).

後処理

  1. temperatureThe mixture was heated
  2. customevaporated to dryness under reduced pressure
  3. dissolutionThe residue was dissolved in water
  4. extractionextracted with ethyl acetate
  5. washThe ethyl acetate layers were washed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. customevaporated to dryness under reduced pressure

出典と根拠

ORDレコード
ord-6347d1f82a064e9f8d32ac54dafecf38
出典データセット
uspto-grants-1982_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04356186

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート