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4-Amino-1-Boc-piperidine → 1,1-Dimethylethyl 4-[[4-amino-5-(2,3-difluoro-6-methoxybenzoyl)-2-pyrimidinyl]amino]-1-piperidinecarboxylate

HRID 1435248
ノート
印刷プレビュー

反応式

HRID 1435248 の反応式
[NH2:1][C:2]1[C:7]([C:8]([C:10]2[C:15]([O:16][CH3:17])=[CH:14][CH:13]=[C:12]([F:18])[C:11]=2[F:19])=[O:9])=[CH:6][N:5]=[C:4](S(CC)=O)[N:3]=1.[NH2:24][CH:25]1[CH2:30][CH2:29][N:28]([C:31]([O:33][C:34]([CH3:37])([CH3:36])[CH3:35])=[O:32])[CH2:27][CH2:26]1>CN1CCCC1=O.O>[C:34]([O:33][C:31]([N:28]1[CH2:29][CH2:30][CH:25]([NH:24][C:4]2[N:3]=[C:2]([NH2:1])[C:7]([C:8](=[O:9])[C:10]3[C:15]([O:16][CH3:17])=[CH:14][CH:13]=[C:12]([F:18])[C:11]=3[F:19])=[CH:6][N:5]=2)[CH2:26][CH2:27]1)=[O:32])([CH3:37])([CH3:35])[CH3:36]
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 2

HCID 12682914-Amino-1-Boc-piperidineHCID 21070554(4-Amino-2-(ethylsulfinyl)pyrimidin-5-yl)(2,3-difluoro-6-methoxyphenyl)methanone

生成物 1

HCID 587775881,1-Dimethylethyl 4-[[4-amino-5-(2,3-difluoro-6-methoxybenzoyl)-2-pyrimidinyl]amino]-1-piperidinecarboxylate収率 80%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 13387
N-methyl-2-pyrrolidone
溶媒

実験手順

A solution of (4-amino-2-ethanesulfinyl-pyrimidin-5-yl)-(2,3-difluoro-6-methoxy-phenyl)-methanone (7.7 g, 23 mmol, Example 165) and 4-amino-1N-Boc-piperidine (6.8 g, 34 mmol, Astatech) in 30 mL of 1-methyl-2-pyrrolidinone was heated at 70° C. for 30 minutes. The reaction mixture was diluted with water and extracted with ethyl acetate. The dried (Na2SO4) organic solution was evaporated and the residue was chromatographed on silica gel. Elution with 3:2 ethyl acetate/hexane provided 80% yield of 4-[4-amino-5-(2,3-difluoro-6-methoxy-benzoyl)-pyrimidin-2-ylamino]-piperidine-1-carboxylic acid tert-butyl ester as a colorless solid, mp 114 dec., identical to material prepared in Example 106. Mass Spectrum (LR-ES) M+: 463.

後処理

  1. extractionextracted with ethyl acetate
  2. dry with materialThe dried (Na2SO4) organic solution
  3. customwas evaporated
  4. customthe residue was chromatographed on silica gel
  5. washElution with 3:2 ethyl acetate/hexane

出典と根拠

ORDレコード
ord-21842b7281274579804a3a0ef377cb77
出典データセット
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07615634B2

反応ノート

読み込み中…

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