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Methanol → 2,2-Diphenyloxirane

HRID 1683356
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HRID 1683356 반응식
S(=O)(=O)(O)O.CSC.CO.[C:11](O)(C)(C)C.[C:16]([C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)(=[O:23])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.[OH-].[K+]>>[C:17]1([C:16]2([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)[O:23][CH2:11]2)[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 6

HCID 887MethanolHCID 1068Dimethyl SulfideHCID 1118Sulfuric AcidHCID 3102BenzophenoneHCID 6386tert-ButanolHCID 14797Potassium Hydroxide

생성물 1

HCID 935642,2-Diphenyloxirane

실험 절차

Sulphuric acid (23.7 g at 98%, 0.237 moles) was added dropwise, with stirring, to dimethylsulphide (20.0 g at 98%, 0.316 moles) over 60 minutes, maintaining the temperature below 26° C. Methanol (5.0 g, 0.156 mole) was added slowly to the stirred mixture maintaining the temperature below 31° C. The reaction mixture was stirred for 41/2 hours and head overnight unagitated at room temperature. Tertiary butanol (3.6 g, 0.048 mole) and benzophenone (27.4 g, 0.15 mole) were added to the reaction mixture. Potassium hydroxide flake (43.4 g, 0.73 mole) was added in 10 equal aliquots over 3 hours while maintaining the temperature below 40° C. The reaction was monitored by GC and then stirred overnight at room temperature.

후처리

  1. temperaturemaintaining the temperature below 26° C
  2. temperaturemaintaining the temperature below 31° C
  3. waithead overnight unagitated at room temperature
  4. temperaturewhile maintaining the temperature below 40° C
  5. stirringstirred overnight at room temperature

출처 및 근거

ORD 기록
ord-7377de9cb3384830a45c128508eb003c
출처 데이터셋
uspto-grants-1997_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05637727

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