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

HRID 1006454

反応式

HRID 1006454 の反応式
[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

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-4747734e55d94db39ad7b3f4b52ddef0
出典データセット
uspto-grants-2004_09
特許番号
US06790865B2

関連ノート

読み込み中…