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4-Isopropylbenzenethiol → HCID 20985432、化合物

HRID 1518205
ノート
印刷プレビュー

反応式

HRID 1518205 の反応式
[CH:1]([C:4]1[CH:9]=[CH:8][C:7]([SH:10])=[CH:6][CH:5]=1)([CH3:3])[CH3:2].Br[CH2:12][C:13]1[CH:18]=[CH:17][C:16]([CH2:19][C:20]([OH:22])=[O:21])=[CH:15][CH:14]=1>CN(C)C=O>[CH:1]([C:4]1[CH:9]=[CH:8][C:7]([S:10][CH2:12][C:13]2[CH:14]=[CH:15][C:16]([CH2:19][C:20]([OH:22])=[O:21])=[CH:17][CH:18]=2)=[CH:6][CH:5]=1)([CH3:3])[CH3:2]
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 5212514-IsopropylbenzenethiolHCID 45190564-(Bromomethyl)phenylacetic acid

生成物 1

HCID 20985432HCID 20985432、化合物収率 99%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

To a solution of 4-(isopropyl)thiophenol (10 g, 65.68 mmol) in N,N-dimethylformamide (200 ml) sodium hydride (3.15 g, 131.35 mmol) was added. The exothermic reaction was allowed to cool down to room temperature. At 15° C. a solution of (4-bromomethyl-phenyl)-acetic acid (15.04 g, 65.68 mmol) in N,N-dimethylformamide (100 ml) was added. After stirring the reaction mixture at room temperature for 16 h the mixture was concentrated, diluted with water, and adjusted to pH=2 by adding HCl (2N). The aqueous phase was extracted three times with ethyl acetate. The combined organic layers were dried over MgSO4, filtered, and the solvent evaporated under reduced pressure to give the product as a yellow oil (19.5 g, 99%).

後処理

  1. customThe exothermic reaction
  2. concentrationwas concentrated
  3. additiondiluted with water
  4. additionby adding HCl (2N)
  5. extractionThe aqueous phase was extracted three times with ethyl acetate
  6. dry with materialThe combined organic layers were dried over MgSO4
  7. filtrationfiltered
  8. customthe solvent evaporated under reduced pressure

出典と根拠

ORDレコード
ord-197bed3c647744828ab5518f529ad3f3
出典データセット
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08232426B2

反応ノート

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