Water → tert-Butyl [2-(5-oxo-4,5-dihydro[1,3,4]oxadiazol-2-yl)thiophen-3-yl]carbamate

HRID 460314노트

반응식

HRID 460314 반응식
[C:1](Cl)(Cl)=[O:2].[C:5]([O:9][C:10]([NH:12][C:13]1[CH:17]=[CH:16][S:15][C:14]=1[C:18]([NH:20][NH2:21])=[O:19])=[O:11])([CH3:8])([CH3:7])[CH3:6].O>C1COCC1>[O:2]=[C:1]1[O:19][C:18]([C:14]2[S:15][CH:16]=[CH:17][C:13]=2[NH:12][C:10](=[O:11])[O:9][C:5]([CH3:8])([CH3:6])[CH3:7])=[N:20][NH:21]1

참가 물질

5

반응물 3

HCID 962WaterHCID 6371PhosgeneHCID 184459443-(tert-Butoxycarbonylamino)thiophene-2-carboxylic hydrazide

생성물 1

HCID 86760474tert-Butyl [2-(5-oxo-4,5-dihydro[1,3,4]oxadiazol-2-yl)thiophen-3-yl]carbamate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

4 ml of a 20% toluenic phosgene solution are added dropwise to a solution of 240 mg of 3-(tert-butoxycarbonylamino)thiophene-2-carboxylic hydrazide in 5 ml of THF and the mixture is stirred at RT. After one hour, the mixture is admixed with 10 ml of water and, after brief digestion, extracted with ethyl acetate. After the ethyl acetate phase has been dried over sodium sulfate, the mixture is concentrated under reduced pressure and the remaining residue is used further without further purification.

후처리

  1. extractionafter brief digestion, extracted with ethyl acetate
  2. dry with materialAfter the ethyl acetate phase has been dried over sodium sulfate
  3. concentrationthe mixture is concentrated under reduced pressure
  4. customthe remaining residue is used further without further purification

출처 및 근거

ORD 기록
ord-37189ac45f724e52911353c37347c860
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07196114B2

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