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Ammonia → HCID 178449126, 화합물

HRID 1285569
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HRID 1285569 반응식
[C:1]([NH:5][CH2:6][CH:7]([OH:25])[CH2:8][O:9][C:10]1[CH:15]=[CH:14][C:13]([C:16]2[NH:17][CH:18]=[C:19]([C:21]([O:23]C)=O)[N:20]=2)=[CH:12][CH:11]=1)([CH3:4])([CH3:3])[CH3:2].[NH3:26]>CO>[C:1]([NH:5][CH2:6][CH:7]([OH:25])[CH2:8][O:9][C:10]1[CH:15]=[CH:14][C:13]([C:16]2[NH:17][CH:18]=[C:19]([C:21](=[O:23])[NH2:26])[N:20]=2)=[CH:12][CH:11]=1)([CH3:4])([CH3:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 222AmmoniaHCID 178498876HCID 178498876, 화합물

생성물 1

HCID 178449126HCID 178449126, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of methyl 2-[4-(3-tert. butylamino-2-hydroxypropoxy)phenyl]imidazole-4-carboxylate (10 g.) in methanol (100 ml.) is reacted in a bomb with ammonia (44 g.) at 100° C. for 24 hours. The reaction mixture is concentrated under reduced pressure and the residue is chromatographed on silica gel. The product is eluted with chloroform that is washed with concentrated aqueous ammonia (90%) and methanol (10%) and is recrystallized from acetonitrile to yield the 2-[4-(3-tert. butylamino-2-hydroxypropoxy)phenyl]-4-carbamoylimidazole as a white solid, m.p. 149°-154° C.

후처리

  1. concentrationThe reaction mixture is concentrated under reduced pressure
  2. customthe residue is chromatographed on silica gel
  3. washThe product is eluted with chloroform that
  4. washis washed with concentrated aqueous ammonia (90%) and methanol (10%)
  5. customis recrystallized from acetonitrile

출처 및 근거

ORD 기록
ord-d4a046a1ad1d4968ab67705a6cb68d68
출처 데이터셋
uspto-grants-1986_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04567276

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