(1-Bromo-2,2-dimethylpropyl)benzene → HCID 87316481, 화합물

HRID 1844379노트

반응식

HRID 1844379 반응식
Br[CH:2]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)[C:3]([CH3:6])([CH3:5])[CH3:4].[C:13]([O-:16])(=[S:15])[CH3:14].[K+]>CN(C=O)C>[CH3:4][C:3]([CH3:6])([CH3:5])[CH:2]([S:15][C:13](=[O:16])[CH3:14])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

참가 물질

4

반응물 2

HCID 14912426(1-Bromo-2,2-dimethylpropyl)benzeneHCID 23670855Potassium ethanethioate

생성물 1

HCID 87316481HCID 87316481, 화합물수율 99.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
50 °C

실험 절차

(1-Bromo-2,2-dimethyl-propyl)-benzene (1.00 g, 4.40 mmol) was dissolved in dry DMF (5 mL) under an argon atmosphere. Potassium thioacetate (2.51 g, 22.0 mmol) was added and the reaction was heated to 50° C. for 7 days. The solution was then concentrated and the product purified by column chromatography to obtain the desired thioester (970 mg, 99%). TLC (Hexane:CH2Cl2, 7:3 v/v): Rf=0.40. 1H NMR (400 MHz, CDCl3): δ 7.33-7.22 (m, 5H), 4.52 (s, 1H), 2.32 (s, 3H), 1.00 (s, 9H). 13C NMR (100 MHz, CDCl3): δ 193.9 (q), 140.4 (q), 129.0, 127.2, 126.4, 58.7, 34.9 (q), 30.2, 27.6. HRMS (m/z): [M+Na]+ calcd. for C13H18ONaS 245.0976; found, 245.0972.

후처리

  1. concentrationThe solution was then concentrated
  2. customthe product purified by column chromatography

출처 및 근거

ORD 기록
ord-75eafea52e424fd195bda8cfc61eaa40
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08946429B2

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