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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
ノート
印刷プレビュー

反応式

HRID 82258 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran
溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-a1a9372cbdb047b5b5815df22e7e8239
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08846698B2

反応ノート

読み込み中…

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