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Methanol → 2,2-Diphenyloxirane

HRID 1683356
ノート
印刷プレビュー

反応式

HRID 1683356 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 6

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

生成物 1

HCID 935642,2-Diphenyloxirane

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7377de9cb3384830a45c128508eb003c
出典データセット
uspto-grants-1997_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05637727

反応ノート

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