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

HRID 971219노트

반응식

HRID 971219 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
180 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-516e1152c3be4900a1b97a1d5f54389c
출처 데이터셋
uspto-grants-2007_12
특허 번호
US07312330B2

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