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4-Isopropylbenzenethiol → HCID 20985432, 화합물

HRID 1518205
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HRID 1518205 반응식
[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]
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참가 물질

4

반응물 2

HCID 5212514-IsopropylbenzenethiolHCID 45190564-(Bromomethyl)phenylacetic acid

생성물 1

HCID 20985432HCID 20985432, 화합물수율 99%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-197bed3c647744828ab5518f529ad3f3
출처 데이터셋
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08232426B2

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