Water → Benzyl 4'-(2-methanesulfonyloxy-ethoxy)-3'5'-dimethylbiphenyl-4-carboxylate

HRID 2243543노트

반응식

HRID 2243543 반응식
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[OH:6][CH2:7][CH2:8][O:9][C:10]1[C:15]([CH3:16])=[CH:14][C:13]([C:17]2[CH:22]=[CH:21][C:20]([C:23]([O:25][CH2:26][C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)=[O:24])=[CH:19][CH:18]=2)=[CH:12][C:11]=1[CH3:33].C(N(CC)CC)C.O>C(Cl)Cl.C(OCC)(=O)C>[CH3:1][S:2]([O:6][CH2:7][CH2:8][O:9][C:10]1[C:11]([CH3:33])=[CH:12][C:13]([C:17]2[CH:22]=[CH:21][C:20]([C:23]([O:25][CH2:26][C:27]3[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=3)=[O:24])=[CH:19][CH:18]=2)=[CH:14][C:15]=1[CH3:16])(=[O:4])=[O:3]

참가 물질

7

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 23090745Benzyl 4'-(2-hydroxyethoxy)-3',5'-dimethylbiphenyl-4-carboxylate

생성물 1

HCID 23090786Benzyl 4'-(2-methanesulfonyloxy-ethoxy)-3'5'-dimethylbiphenyl-4-carboxylate

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매

실험 절차

Methanesulfonyl chloride (0.10 mL) was added to an ice-cooled mixture of benzyl 4′-(2-hydroxy-ethoxy)-3′,5′-dimethylbiphenyl-4-carboxylate (0.38 g) and triethylamine (0.21 mL) in methylene chloride (5 mL) with stirring, and the mixture was stirred at room temperature for 1 hr. Water and ethyl acetate were added to the reaction mixture. The organic layer was separated, washed with water and brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure to afford benzyl 4′-(2-methanesulfonyloxy -ethoxy)-3′5′-dimethylbiphenyl-4-carboxylate (0.45 g).

후처리

  1. temperaturecooled
  2. stirringthe mixture was stirred at room temperature for 1 hr
  3. customThe organic layer was separated
  4. washwashed with water and brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-f420e5c56cee4f16b7465ad1868bfa1e
출처 데이터셋
uspto-grants-2010_03
특허 번호
US07674938B2

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