Isopropenyl chloroformate → Prop-1-en-2-yl (2-fluoro-4-methyl-5-(7-methyl-2-(methylamino)pyrido[2,3-d]pyrimidin-6-yl)phenyl)carbamate

HRID 522728ノート

反応式

HRID 522728 の反応式
[NH2:1][C:2]1[C:3]([F:22])=[CH:4][C:5]([CH3:21])=[C:6]([C:8]2[C:19]([CH3:20])=[N:18][C:11]3[N:12]=[C:13]([NH:16][CH3:17])[N:14]=[CH:15][C:10]=3[CH:9]=2)[CH:7]=1.Cl[C:24]([O:26][C:27]([CH3:29])=[CH2:28])=[O:25]>N1C=CC=CC=1>[F:22][C:3]1[CH:4]=[C:5]([CH3:21])[C:6]([C:8]2[C:19]([CH3:20])=[N:18][C:11]3[N:12]=[C:13]([NH:16][CH3:17])[N:14]=[CH:15][C:10]=3[CH:9]=2)=[CH:7][C:2]=1[NH:1][C:24](=[O:25])[O:26][C:27]([CH3:29])=[CH2:28]

参加物

4

反応物 2

HCID 93846Isopropenyl chloroformateHCID 898135606-(5-Amino-4-fluoro-2-methylphenyl)-N,7-dimethylpyrido[2,3-d]pyrimidin-2-amine

生成物 1

HCID 118048014Prop-1-en-2-yl (2-fluoro-4-methyl-5-(7-methyl-2-(methylamino)pyrido[2,3-d]pyrimidin-6-yl)phenyl)carbamate収率 100%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
0 °C

実験手順

Treat a cooled solution (0° C.) of 6-(5-amino-4-fluoro-2-methylphenyl)-N,7-dimethylpyrido[2,3-d]pyrimidin-2-amine (0.85 g, 2.86 mmol) in pyridine (10 mL) dropwise with isopropenyl chloroformate (0.281 ml, 2.57 mmol) and stir the mixture for 20 min. at 0° C. Concentrate the mixture to dryness, dissolve the residue in DCM, wash with brine, dry over Na2SO4 and concentrate to dryness to afford the title compound. Use it without purification (assuming 100% yield). MS (m/z): 382.1 (M+1).

後処理

  1. concentrationConcentrate the mixture to dryness
  2. dissolutiondissolve the residue in DCM
  3. washwash with brine
  4. dry with materialdry over Na2SO4
  5. concentrationconcentrate to dryness

出典と根拠

ORDレコード
ord-38ce905859d74b3baf6a9dc752227a7a
出典データセット
uspto-grants-2016_05
特許番号
US09334267B2

反応ノート

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