Potassium Carbonate → 1-Adamantyl 3,4-dichlorophenylthiomethyl ketone

HRID 259309

反応式

HRID 259309 の反応式
Br[CH2:2][C:3]([C:5]12[CH2:14][CH:9]3[CH2:10][CH:11]([CH2:13][CH:7]([CH2:8]3)[CH2:6]1)[CH2:12]2)=[O:4].[Cl:15][C:16]1[CH:17]=[C:18]([SH:23])[CH:19]=[CH:20][C:21]=1[Cl:22].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[Cl:15][C:16]1[CH:17]=[C:18]([S:23][CH2:2][C:3]([C:5]23[CH2:14][CH:9]4[CH2:10][CH:11]([CH2:13][CH:7]([CH2:8]4)[CH2:6]2)[CH2:12]3)=[O:4])[CH:19]=[CH:20][C:21]=1[Cl:22]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 799643,4-DichlorobenzenethiolHCID 197820Bromomethyl tricyclo[3.3.1.13,7]dec-1-yl ketone

生成物 1

HCID 214240441-Adamantyl 3,4-dichlorophenylthiomethyl ketone

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

1-adamantyl bromomethyl ketone (1.3 g.), 1.1 g. of 3,4-dichlorothiophenol and 800 mg. of anhydrous potassium carbonate in 30 ml. of acetone are stirred at reflux overnight. The solvent is then removed and 60 ml. of water is added to the reaction mixture. The product is filtered off, washed with water and recrystallized from methanol to yield 1-adamantyl 3,4-dichlorophenylthiomethyl ketone, M.P. 105°-110.5° C.

後処理

  1. temperatureat reflux overnight
  2. customThe solvent is then removed
  3. additionof water is added to the reaction mixture
  4. filtrationThe product is filtered off
  5. washwashed with water
  6. customrecrystallized from methanol

出典と根拠

ORDレコード
ord-5fa6384611b3406fa60c6e11270986ca
出典データセット
uspto-grants-1977_07
特許番号
US04036975

関連ノート

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