Water → HCID 68643629、化合物

HRID 1158200ノート

反応式

HRID 1158200 の反応式
C[O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[S:17][CH3:18])=[O:10].[Al+3].[Cl-].[Cl-].[Cl-].C(S)CCCCCCCCCCC.O>CCCCCC.C(OCC)(=O)C>[OH:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[S:17][CH3:18])=[O:10]

参加物

6

反応物 4

HCID 962WaterHCID 81951-DodecanethiolHCID 6451240Aluminum(III) ChlorideHCID 247227562-Methoxy-2'-thiomethylbenzophenone

生成物 1

HCID 68643629HCID 68643629、化合物収率 60%

試薬・触媒・溶媒 1

HCID 21226206Ethyl acetate hexane溶媒

実験手順

To a mixture of 1.45 g (2-methoxyphenyl)(2-(methylthio)phenyl)methanone (G) and 1.437 g AlCl3 was added slowly 5 mL 1-dodecanethiol. The reaction was stirred overnight before 30 ml water was added. The mixture was extracted with ethyl acetate and the combined organic extracts were washed with brine, dried over magnesium sulfate, and the volatiles removed by distillation under nitrogen. Flash silica chromatography (hexane:ethyl acetate 80:20) afforded 0.807 g product (3.31 mmol, 60% yield).

後処理

  1. additionwas added
  2. extractionThe mixture was extracted with ethyl acetate
  3. washthe combined organic extracts were washed with brine
  4. dry with materialdried over magnesium sulfate
  5. customthe volatiles removed by distillation under nitrogen

出典と根拠

ORDレコード
ord-6e1ef128ff5944eb8f20b504429156d4
出典データセット
uspto-grants-2010_10
特許番号
US07807713B2

反応ノート

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