Hydrochloric Acid → HCID 19855336, 화합물

HRID 1650066

반응식

HRID 1650066 반응식
[C:1]1([S:7](OC)=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[H-].[K+].[CH3:13][C@H:14]1[C@H:19]([CH2:20][CH:21]=[CH2:22])[CH2:18][CH2:17][C:16](=[O:23])[CH2:15]1.Cl>C(COC)OC>[CH3:13][CH:14]1[CH2:15][C:16](=[O:23])[CH:17]([S:7][C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[CH2:18][CH:19]1[CH2:20][CH:21]=[CH2:22]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 82127Potassium hydrideHCID 2759784Methyl benzenesulfinateHCID 15670663(3R,4S)-3-Methyl-4-(prop-2-en-1-yl)cyclohexan-1-one

생성물 1

HCID 19855336HCID 19855336, 화합물

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매2회

반응 조건

온도
0 °C

실험 절차

To a 0° C. mixture of 16.9 g. (0.109 mole) of methyl benzenesulfinate and 8.68 g. (0.217 mole) of potassium hydride in 100 ml. of dimethoxyethane was slowly added a solution of 15.0 g. (0.0987 mole) of trans-3-methyl-4-(2-propenyl)cyclohexanone in 50 ml. of dimethoxyethane. The reaction was stirred 30 minutes longer at 0° C. and then cautiously added to 500 ml. of ice-saturated sodium chloride and 45 ml. 6N hydrochloric acid. The quenched reaction mixture was extracted once with 300 ml. ether and once with 200 ml. dichloromethane. The organic extract was dried over magnesium sulfate and evaporated to give a quantitative yield of the title compound as a semisolid mixture of axial and equatorial sulfenates. Crystallization from ether yields 7.8 g. of pure axial sulfenate.

후처리

  1. additionTo a 0° C. mixture of 16.9 g
  2. additioncautiously added to 500 ml
  3. customThe quenched reaction mixture
  4. extractionwas extracted once with 300 ml
  5. extractionThe organic extract
  6. dry with materialwas dried over magnesium sulfate
  7. customevaporated
  8. customto give

출처 및 근거

ORD 기록
ord-e3ba299f00b44733bd756c1fc9a27b05
출처 데이터셋
uspto-grants-1990_05
특허 번호
US04921994

연결된 노트

불러오는 중…