Sodium Bicarbonate → HCID 21941354, 화합물

HRID 1158850노트

반응식

HRID 1158850 반응식
F[B-](F)(F)F.C[O+:7]([CH3:9])[CH3:8].[N+:10]([C:13]1[CH:29]=[CH:28][C:16]([CH2:17][O:18][C:19]([N:21]2C[CH2:25][NH:24][C:23](=O)[CH2:22]2)=[O:20])=[CH:15][CH:14]=1)([O-:12])=[O:11].C(=O)([O-])O.[Na+]>ClCCl>[CH3:8][O:7][CH:9]1[CH2:25][NH:24][CH2:23][CH2:22][N:21]1[C:19]([O:18][CH2:17][C:16]1[CH:15]=[CH:14][C:13]([N+:10]([O-:12])=[O:11])=[CH:29][CH:28]=1)=[O:20]

참가 물질

5

반응물 3

HCID 516892Sodium BicarbonateHCID 2735153Oxonium, trimethyl-, tetrafluoroborate(1-) (1:1)HCID 21941454(4-Nitrophenyl)methyl 3-oxo-1-piperazinecarboxylate

생성물 1

HCID 21941354HCID 21941354, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Trimethyloxonium tetrafluoroborate (97%, 3.7 g) was added to the dry dichloromethane (120 mL) solution of 4-p-nitrobenzyloxycarbonyl-2-oxopiperazine (6.7 g) at room temperature and stirred for 17 hours. The reaction mixture was treated with saturated sodium hydrogen carbonate aqueous solution, and the organic layer was separated. The aqueous layer was extracted with ethyl acetate (3×100 mL), then the combined organic layer was washed with saturated sodium hydrogen carbonate aqueous solution and brine. The organic layer was dried (MgSO4) and filtered. The filtrate was concentrated under reduce pressure and the title compound was obtained as a pale brown solid. Yield; 5.7 g, 80.6.

후처리

  1. customthe organic layer was separated
  2. extractionThe aqueous layer was extracted with ethyl acetate (3×100 mL)
  3. washthe combined organic layer was washed with saturated sodium hydrogen carbonate aqueous solution and brine
  4. dry with materialThe organic layer was dried (MgSO4)
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated

출처 및 근거

ORD 기록
ord-4681d1050260473ab4cb4df3e68951ae
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07812014B2

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