Ammonia → HCID 178501028, 화합물

HRID 2391737노트

반응식

HRID 2391737 반응식
Cl.Cl.[NH:3]1[C:11]2[CH2:10][C@@H:9]([C:12]([O:14][CH3:15])=[O:13])[NH:8][CH2:7][C:6]=2[N:5]=[CH:4]1.N.CO>ClCCl>[NH:3]1[C:11]2[CH2:10][C@@H:9]([C:12]([O:14][CH3:15])=[O:13])[NH:8][CH2:7][C:6]=2[N:5]=[CH:4]1

참가 물질

5

반응물 3

HCID 222AmmoniaHCID 887MethanolHCID 178501029HCID 178501029, 화합물

생성물 1

HCID 178501028HCID 178501028, 화합물수율 95.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Into a mixture of 188.25 g methyl (65)-4,5,6,7-tetrahydro-imidazo[4,5-c]pyridine-6-carboxylate dihydrochloride in 3 l dichloromethane at 10-15° C. is lead gaseous ammonia until saturation takes place (about one hour). 200 ml methanol are added and the mixture is filtered. The filter cake is washed with 2×100 ml DCM/MeOH (8/2 v/v). The filtrate is concentrated under reduced pressure and the resulting solid is dried under vacuum to give 128.4 g of the title product.

후처리

  1. customplace (about one hour)
  2. filtrationthe mixture is filtered
  3. washThe filter cake is washed with 2×100 ml DCM/MeOH (8/2 v/v)
  4. concentrationThe filtrate is concentrated under reduced pressure
  5. customthe resulting solid is dried under vacuum

출처 및 근거

ORD 기록
ord-dd86a1f0dfc44962ae48d5e8aeee343e
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08273890B2

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