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Trichloroethylene → HCID 23681230、化合物

HRID 1532922
ノート
印刷プレビュー

反応式

HRID 1532922 の反応式
[CH3:1][C:2]1[CH:3]=[N:4][C:5]([CH2:11][S+:12]([O-:24])[C:13]2[NH:14][C:15]3[CH:16]=[CH:17][C:18]([O:22][CH3:23])=[CH:19][C:20]=3[N:21]=2)=[C:6]([CH3:10])[C:7]=1[O:8][CH3:9].[OH-:25].[Na+:26].ClC=C(Cl)Cl>O1CCCC1>[CH3:1][C:2]1[C:7]([O:8][CH3:9])=[C:6]([CH3:10])[C:5]([CH2:11][S:12]([C:13]2[N-:14][C:15]3[CH:16]=[CH:17][C:18]([O:22][CH3:23])=[CH:19][C:20]=3[N:21]=2)=[O:24])=[N:4][CH:3]=1.[OH2:25].[Na+:26]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6575TrichloroethyleneHCID 14798Sodium HydroxideHCID 178488147HCID 178488147、化合物

生成物 1

HCID 23681230HCID 23681230、化合物収率 95%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Omeprazole (1300 g; 3.77 mol) was added under vigorous mechanical stirring to a mixture of tetrahydrofurane (13 L) and 50% aqueous NaOH (296 g, 3.7 mol) and stirring was continued for 45 min. Trichloroethylene (5.7 L) was added and stirring was continued over night at room temperature. The mixture was cooled to +5° C. and then stirred for 3 h. The precipitate was filtered off and the filter cake was washed with trichloroethylene (5 L) and dried under reduced pressure at 50° C. giving omeprazole sodium salt (1314 g, 95%), m.p. 208-210 ° C.

後処理

  1. stirringstirring
  2. waitwas continued over night at room temperature
  3. temperatureThe mixture was cooled to +5° C.
  4. stirringstirred for 3 h
  5. filtrationThe precipitate was filtered off
  6. washthe filter cake was washed with trichloroethylene (5 L)
  7. customdried under reduced pressure at 50° C.

出典と根拠

ORDレコード
ord-3a34c67e91a04c1f8ecac679be2aa99c
出典データセット
uspto-grants-2001_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06207188B1

反応ノート

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