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

HRID 259309

반응식

HRID 259309 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 214240441-Adamantyl 3,4-dichlorophenylthiomethyl ketone

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5fa6384611b3406fa60c6e11270986ca
출처 데이터셋
uspto-grants-1977_07
특허 번호
US04036975

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