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Potassium Carbonate → HCID 13827615、化合物

HRID 235672
ノート
印刷プレビュー

反応式

HRID 235672 の反応式
[CH:1]1([C:6]2([CH3:19])[CH2:14][C:13]3[C:8](=[C:9]([Cl:17])[C:10]([Cl:16])=[C:11](O)[CH:12]=3)[C:7]2=[O:18])[CH2:5][CH2:4][CH2:3][CH2:2]1.C(=O)([O-])[O-].[K+].[K+].FC(F)(F)[S:28](Cl)(=O)=O>CC(C)=O>[CH:1]1([C:6]2([CH3:19])[CH2:14][C:13]3[C:8](=[C:9]([Cl:17])[C:10]([Cl:16])=[C:11]([SH:28])[CH:12]=3)[C:7]2=[O:18])[CH2:5][CH2:4][CH2:3][CH2:2]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 79000Trifluoromethanesulfonyl chlorideHCID 123955886,7-Dichloro-2-cyclopentyl-5-hydroxy-2-methylindan-1-one

生成物 1

HCID 13827615HCID 13827615、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

反応条件

温度
0 °C

実験手順

To a solution of 600 mg of (2RS)-2-cyclopentyl-2-methyl-5-hydroxy-6,7-dichloroindan-1-one (prepared by the method described in European Patent Publication No. 47011) in 6 ml of dry acetone was added 690 mg of potassium carbonate at a time and the mixture was stirred for twenty minutes. The reaction mixture was cooled to 0° C., 0.23 ml of trifluoromethanesulfonyl chloride was dropped thereto and the mixture was stirred for 10 minutes at the same temperature. The solid was filtered out from the reaction mixture and the filtrate was concentrated under reduced pressure. The obtained residue was dissolved in methylene chloride and the solution was dried over anhydrous magnesium sulfate and concentrated under reduced pressure to give 860 mg of the title compound as crude product having the following physical data.

後処理

  1. stirringthe mixture was stirred for 10 minutes at the same temperature
  2. filtrationThe solid was filtered out from the reaction mixture
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. dissolutionThe obtained residue was dissolved in methylene chloride
  5. dry with materialthe solution was dried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-d87b8076768a42a2b6f35d56ff7a794b
出典データセット
uspto-grants-1987_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04640931

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート