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

HRID 2243543ノート

反応式

HRID 2243543 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-f420e5c56cee4f16b7465ad1868bfa1e
出典データセット
uspto-grants-2010_03
特許番号
US07674938B2

反応ノート

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