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Water → HCID 20075597, 화합물

HRID 704139
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HRID 704139 반응식
[CH2:1]([CH:5]([C:11]([O:13][CH2:14][CH3:15])=[O:12])[C:6]([O:8][CH2:9][CH3:10])=[O:7])[CH:2]([CH3:4])[CH3:3].[H-].[Na+].Cl[CH2:19][S:20][CH2:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1.O>C1(C)C=CC=CC=1>[CH2:21]([S:20][CH2:19][C:5]([CH2:1][CH:2]([CH3:4])[CH3:3])([C:11]([O:13][CH2:14][CH3:15])=[O:12])[C:6]([O:8][CH2:9][CH3:10])=[O:7])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 25047Diethyl isobutylmalonateHCID 319930Benzyl Chloromethyl Sulfide

생성물 1

HCID 20075597HCID 20075597, 화합물수율 98%

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

Diethyl isobutylmalonate (22.0 g.) was added to a stirred suspension of sodium hydride (4.8 g. 50% dispersion in oil) in dry toluene (200 ml.), under nitrogen. The mixture was stirred at 80° for one hour. The mixture was cooled and benzyl chloromethyl thioether 5 (16.0 g.) in dry toluene (50 ml.) was added and the mixture was stirred at 80° for two hours. The mixture was cooled and poured into water. The aqueous mixture was extracted into diethyl ether. The ether extracts were washed with water, dried over anhydrous magnesium sulphate and evaporated in vacuo. Diethyl 2-benzylthiomethyl-2-isobutylmalonate (32.0 g.) was obtained as a yellow oil and was used without further purification.

후처리

  1. temperatureThe mixture was cooled
  2. stirringthe mixture was stirred at 80° for two hours
  3. temperatureThe mixture was cooled
  4. extractionThe aqueous mixture was extracted into diethyl ether
  5. washThe ether extracts were washed with water
  6. dry with materialdried over anhydrous magnesium sulphate
  7. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-439d5bfe21af4a6582326cacfb56f26a
출처 데이터셋
uspto-grants-1991_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04985582

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