tert-Butyl mercaptan → HCID 54548855, 화합물

HRID 1979805노트

반응식

HRID 1979805 반응식
Cl[CH:2]=[C:3]([Cl:7])[C:4](=[O:6])[CH3:5].[C:8]([SH:12])([CH3:11])([CH3:10])[CH3:9].C(N(CC)CC)C>C(OCC)C>[Cl:7][C:3]([C:4](=[O:6])[CH3:5])=[CH:2][S:12][C:8]([CH3:11])([CH3:10])[CH3:9]

참가 물질

5

반응물 3

HCID 6387tert-Butyl mercaptanHCID 8471TriethylamineHCID 534251373,4-Dichlorobut-3-en-2-one

생성물 1

HCID 54548855HCID 54548855, 화합물수율 60.7%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

반응 조건

온도
5 °C

실험 절차

To a mixture of 20.85 g (0.15 mole) 1,2-dichloro-1-buten-3-one and 13.53 g (0.15 mole) t-butylmercaptan in 300 ml ethyl ether, cooled to 5° C. is added dropwise 15.18 g (0.15 mole) triethylamine in 50 ml ether. After stirring at room temperature for 18 hours the mixture is heated at reflux for 2 days. The resulting mixture is washed with water, brine and the organic layer dried over magnesium sulfate. Evaporation of ether affords a brown oil which is distilled in vacuo to yield 17.56 g of product as a light yellow liquid, B.P. 75° (0.1 mm) which crystallized upon standing, M.P. 73° C. Mass spectrum (m/e) 192 (molecular ion), 138, 136.

후처리

  1. temperatureis heated
  2. temperatureat reflux for 2 days
  3. washThe resulting mixture is washed with water, brine
  4. dry with materialthe organic layer dried over magnesium sulfate
  5. customEvaporation of ether
  6. customaffords a brown oil which
  7. distillationis distilled in vacuo

출처 및 근거

ORD 기록
ord-e2f1e286b6ce4938839c60a77bcdf552
출처 데이터셋
uspto-grants-1984_11
특허 번호
US04482723

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