Hydrochloric Acid → HCID 19973181, 화합물

HRID 1901288노트

반응식

HRID 1901288 반응식
CC([N:5]([CH2:9][C:10]([NH:12][N:13]1[CH:17]=[CH:16][CH:15]=[C:14]1[C:18](=[O:20])[CH3:19])=[O:11])C(=O)[O-])(C)C.[ClH:21].CCOC(C)=O.CCCCCC>C(OCC)(=O)C.C(O)(C)C>[ClH:21].[C:18]([C:14]1[N:13]([NH:12][C:10](=[O:11])[CH2:9][NH2:5])[CH:17]=[CH:16][CH:15]=1)(=[O:20])[CH3:19]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 21226206Ethyl acetate hexaneHCID 867474421,1-dimethylethyl-[2-[(2-acetyl-1H-pyrrol-1-yl)amino]-2-oxoethyl]carbamate

생성물 1

HCID 19973181HCID 19973181, 화합물

시약·촉매·용매 2

HCID 3776Isopropanol용매HCID 8857Ethyl Acetate용매

실험 절차

To a stirred solution consisting of 1,1-dimethylethyl-[2-[(2-acetyl-1H-pyrrol-1-yl)amino]-2-oxoethyl]carbamate (5.90 g) in ethyl acetate (45 ml) and isopropanol (35ml) was added ethereal HCl (1.7M, excess). The resulting suspension was gently heated until the reaction mixture was homogeneous. After stirring for 24 hours at room temperature, the reaction appeared complete by TLC (silica gel, 50% EtOAc/hexane). The solid product was collected by filtration under nitrogen and recrystallized from methanol/ether to afford 3.30 g of the product, m.p. 179°-182° C.

후처리

  1. temperatureThe resulting suspension was gently heated until the reaction mixture
  2. filtrationThe solid product was collected by filtration under nitrogen
  3. customrecrystallized from methanol/ether

출처 및 근거

ORD 기록
ord-2c00d0da6fa8482a8f73803d2b689126
출처 데이터셋
uspto-grants-1996_11
특허 번호
US05576446

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