Water → Ethyl [4'-(2-methanesulfonyloxy-ethoxy)-2',6'-dimethylbiphenyl-4-yloxy]acetate

HRID 30767노트

반응식

HRID 30767 반응식
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[OH:6][CH2:7][CH2:8][O:9][C:10]1[CH:15]=[C:14]([CH3:16])[C:13]([C:17]2[CH:22]=[CH:21][C:20]([O:23][CH2:24][C:25]([O:27][CH2:28][CH3:29])=[O:26])=[CH:19][CH:18]=2)=[C:12]([CH3:30])[CH:11]=1.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[CH:15]=[C:14]([CH3:16])[C:13]([C:17]2[CH:22]=[CH:21][C:20]([O:23][CH2:24][C:25]([O:27][CH2:28][CH3:29])=[O:26])=[CH:19][CH:18]=2)=[C:12]([CH3:30])[CH:11]=1)(=[O:4])=[O:3]

참가 물질

7

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 86605508HCID 86605508, 화합물

생성물 1

HCID 86605507Ethyl [4'-(2-methanesulfonyloxy-ethoxy)-2',6'-dimethylbiphenyl-4-yloxy]acetate

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매

실험 절차

Methanesulfonyl chloride (0.17 mL) was added to an ice-cooled mixture of ethyl [4′-(2-hydroxyethoxy)-2′,6′-dimethylbiphenyl-4-yloxy]acetate (0.58 g) and triethylamine (0.36 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 ethyl [4′-(2-methanesulfonyloxyethoxy)-2′,6′-dimethylbiphenyl-4-yloxy]acetate.

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-3f759c24098a474d8fb6302bb0a88844
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07423185B2

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