Triethylamine → Ethyl 3-(4-benzyloxyphenyl)-2-methanesulfonyloxypropionate

HRID 1268960노트

반응식

HRID 1268960 반응식
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([CH2:15][CH:16]([OH:22])[C:17]([O:19][CH2:20][CH3:21])=[O:18])=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:23][S:24](Cl)(=[O:26])=[O:25].C(N(CC)CC)C>ClCCl>[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([CH2:15][CH:16]([O:22][S:24]([CH3:23])(=[O:26])=[O:25])[C:17]([O:19][CH2:20][CH3:21])=[O:18])=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 151861533-(4-Benzyloxyphenyl)-2-hydroxypropionic acid ethyl ester

생성물 1

HCID 18625936Ethyl 3-(4-benzyloxyphenyl)-2-methanesulfonyloxypropionate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of ethyl 3-(4-benzyloxyphenyl)lactate (3.32 g) obtained from Reference example 24(a) in anhydrous dichloromethane (30 ml) was added methanesulfonyl chloride (0.94 ml), and then triethylamine (2.47 ml) was added dropwise thereto in an ice bath. The reaction solution was stirred for 3 hours at room temperature and then concentrated under reduced pressure. The residue was partitioned between ethyl acetate and water, and the separated ethyl acetate layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was crystallized from hexane to afford the target compound (3.60 g) as colorless crystals.

후처리

  1. concentrationconcentrated under reduced pressure
  2. customThe residue was partitioned between ethyl acetate and water
  3. dry with materialthe separated ethyl acetate layer was dried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was crystallized from hexane

출처 및 근거

ORD 기록
ord-e5be4514111348399411fa8d41078fdb
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07199139B2

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