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Trichloroethylene → HCID 23681230, 화합물

HRID 1532922
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HRID 1532922 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6575TrichloroethyleneHCID 14798Sodium HydroxideHCID 178488147HCID 178488147, 화합물

생성물 1

HCID 23681230HCID 23681230, 화합물수율 95%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-3a34c67e91a04c1f8ecac679be2aa99c
출처 데이터셋
uspto-grants-2001_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06207188B1

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