Aniline → 7-(3-Chloropyridin-2-yl)-N-(phenyl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidin-4-amine

HRID 971219ノート

反応式

HRID 971219 の反応式
Cl[C:2]1[C:3]2[CH2:11][CH2:10][N:9]([C:12]3[C:17]([Cl:18])=[CH:16][CH:15]=[CH:14][N:13]=3)[CH2:8][C:4]=2[N:5]=[CH:6][N:7]=1.[NH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>C(#N)C>[Cl:18][C:17]1[C:12]([N:9]2[CH2:10][CH2:11][C:3]3[C:2]([NH:19][C:20]4[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=4)=[N:7][CH:6]=[N:5][C:4]=3[CH2:8]2)=[N:13][CH:14]=[CH:15][CH:16]=1

参加物

4

反応物 2

HCID 6115AnilineHCID 590214784-Chloro-7-(3-chloropyridin-2-yl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidine

生成物 1

HCID 120043447-(3-Chloropyridin-2-yl)-N-(phenyl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidin-4-amine収率 32.9%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
180 °C

実験手順

4-Chloro-7-(3-chloro-pyridin-2-yl)-5,6,7,8-tetrahydro-pyrido[3,4-d]pyrimidine (150 mg, 0.54 mmol) was dissolved in acetonitrile (2 mL). To the mixture was added aniline (60 mg). The mixture was heated in a sealed tube at 180° C. for 30 minutes in a Personal Chemistry Microwave (Smith Creator). The solvent was removed under vacuum and the resulting orange residue was purified by flash chromatography over silica gel using a 0-100% ethyl acetate-hexane gradient to give the product as an off white solid (60 mg).

後処理

  1. customThe solvent was removed under vacuum
  2. customthe resulting orange residue was purified by flash chromatography over silica gel using a 0-100% ethyl acetate-hexane gradient

出典と根拠

ORDレコード
ord-516e1152c3be4900a1b97a1d5f54389c
出典データセット
uspto-grants-2007_12
特許番号
US07312330B2

反応ノート

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