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Water → HCID 20148613、化合物

HRID 986437
ノート
印刷プレビュー

反応式

HRID 986437 の反応式
[C:1]([O:4][CH2:5][CH3:6])(=O)[CH3:2].[N:7]1[CH:12]=[CH:11][CH:10]=[C:9]([CH2:13][C:14]2[CH:19]=CC(/C=C/CSCCO)=[CH:16][CH:15]=2)[CH:8]=1.[OH2:27]>>[N:7]1[CH:12]=[CH:11][CH:10]=[C:9]([CH2:13][C:14]2[CH:15]=[CH:16][C:1]([O:4][CH2:5][CH2:6][OH:27])=[CH:2][CH:19]=2)[CH:8]=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 3

HCID 962WaterHCID 8857Ethyl AcetateHCID 15594573HCID 15594573、化合物

生成物 1

HCID 20148613HCID 20148613、化合物収率 89.5%

実験手順

In 3 ml of ethanol was dissolved 310 mg of potassium hydroxide, and 0.37 ml of mercaptoethanol was added to the resulting solution. To this solution was dropwise added the N,N-dimethylformamide solution obtained in (1) above with ice-cooling, and the resulting mixture was subjected to reaction at room temperature for 30 minutes. Subsequently, 30 ml of ethyl acetate and 20 ml of water were added to the reaction mixture, and the organic layer was separated, washed with three 20-ml portions of water, thereafter washed with 20 ml of a saturated aqueous sodium chloride solution, and then dried over anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure to obtain 340 mg (yield 89.5%) of colorless crystals of (E)-2-[3-[4-(pyridin-3-ylmethyl)phenyl]allylthio]ethanol having a melting point of 73°-74° C.

後処理

  1. temperaturecooling
  2. customthe resulting mixture was subjected to reaction at room temperature for 30 minutes
  3. customthe organic layer was separated
  4. washwashed with three 20-ml portions of water
  5. washwashed with 20 ml of a saturated aqueous sodium chloride solution
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customThe solvent was removed by distillation under reduced pressure

出典と根拠

ORDレコード
ord-e41b2bb5e4b247d59a38e94edb2d12d1
出典データセット
uspto-grants-1987_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04713387

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート