Diisopropylethylamine → 4'-[2-(Benzyloxymethoxy)ethyl]-2,2,2-trifluoroacetanilide

HRID 2121846

반응식

HRID 2121846 반응식
[OH:1][CH2:2][CH2:3][C:4]1[CH:16]=[CH:15][C:7]([NH:8][C:9](=[O:14])[C:10]([F:13])([F:12])[F:11])=[CH:6][CH:5]=1.C(N(CC)C(C)C)(C)C.Cl[CH2:27][O:28][CH2:29][C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1>O1CCCC1.ClCCl>[CH2:29]([O:28][CH2:27][O:1][CH2:2][CH2:3][C:4]1[CH:16]=[CH:15][C:7]([NH:8][C:9](=[O:14])[C:10]([F:12])([F:13])[F:11])=[CH:6][CH:5]=1)[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1

참가 물질

6

반응물 3

HCID 81531DiisopropylethylamineHCID 137983Benzyl chloromethyl etherHCID 140791032,2,2-Trifluoro-N-[4-(2-hydroxyethyl)phenyl]acetamide

생성물 1

HCID 226719434'-[2-(Benzyloxymethoxy)ethyl]-2,2,2-trifluoroacetanilide

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매

실험 절차

To a stirred solution of 4′-(2-hydroxyethyl)-2,2,2-trifluoroacetanilide (5.9 g) in tetrahydrofuran (20 ml) and dichloromethane (20 ml) were added N,N-diisopropylethylamine (5.7 ml) and benzyl chloromethyl ether (3.9 ml) under ice-cooling, and the mixture was stirred for 24 hours at room temperature. The reaction mixture was poured into ice-water and extracted with ethyl acetate. The extract was washed with brine and dried over anhydrous magnesium sulfate. Removal of the solvent under reduced pressure gave 4′-[2-(benzyloxymethoxy)ethyl]-2,2,2-trifluoroacetanilide (9.7 g).

후처리

  1. temperaturecooling
  2. extractionextracted with ethyl acetate
  3. washThe extract was washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customRemoval of the solvent under reduced pressure

출처 및 근거

ORD 기록
ord-56f7167509044b64ab4195411a83602c
출처 데이터셋
uspto-grants-2004_02
특허 번호
US06696489B1

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