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Citric Acid → (5-Amino-pyridin-3-yl)-(4-chloro-7-methyl-7H-pyrrolo[2,3-d]pyrimidin-5-yl)-methanone

HRID 82258
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HRID 82258 반응식
C(=[N:14][C:15]1[CH:16]=[C:17]([C:21]([C:23]2[C:31]3[C:30]([Cl:32])=[N:29][CH:28]=[N:27][C:26]=3[N:25]([CH3:33])[CH:24]=2)=[O:22])[CH:18]=[N:19][CH:20]=1)(C1C=CC=CC=1)C1C=CC=CC=1.C(O)(=O)CC(CC(O)=O)(C(O)=O)O.CCOCC>C1COCC1>[NH2:14][C:15]1[CH:16]=[C:17]([C:21]([C:23]2[C:31]3[C:30]([Cl:32])=[N:29][CH:28]=[N:27][C:26]=3[N:25]([CH3:33])[CH:24]=2)=[O:22])[CH:18]=[N:19][CH:20]=1
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참가 물질

5

반응물 3

HCID 311Citric AcidHCID 3283Diethyl EtherHCID 86672119(4-chloro-7-methyl-7H-pyrrolo[2,3-d]pyrimidin-5-yl)(5-((diphenylmethylene)amino)pyridin-3-yl)methanone

생성물 1

HCID 86672120(5-Amino-pyridin-3-yl)-(4-chloro-7-methyl-7H-pyrrolo[2,3-d]pyrimidin-5-yl)-methanone수율 95%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran
용매

실험 절차

A solution of [5-(benzhydrylidene-amino)pyridin-3-yl]-(4-chloro-7-methyl-7H-pyrrolo[2,3-d]pyrimidin-5-yl)-methanone (Preparation 229, 30 g, 0.066 mol) in THF (200 mL) was added aq. citric acid (200 mL), the mixture was stirred for 30 min at room temperature. Ether was added and the layers were separated. The aqueous layer was adjusted to pH7 by aqueous Na2CO3. Then the mixture was filtered. The filter cake was evaporated with toluene and the residue was washed with EtOAc (200 mL) to give the title compound as a brown solid in 95% yield, 18 g.

후처리

  1. customthe layers were separated
  2. filtrationThen the mixture was filtered
  3. customThe filter cake was evaporated with toluene
  4. washthe residue was washed with EtOAc (200 mL)

출처 및 근거

ORD 기록
ord-a1a9372cbdb047b5b5815df22e7e8239
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08846698B2

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