Sodium hydride → 2-Amino-4-(cyclopropylmethyloxy)-6-(4-fluorophenyl)pyrido[3,2-d]pyrimidine

HRID 1517434노트

반응식

HRID 1517434 반응식
C([NH:4][C:5]1[N:6]=[C:7](C2N=CNN=2)[C:8]2[N:14]=[C:13]([C:15]3[CH:20]=[CH:19][C:18]([F:21])=[CH:17][CH:16]=3)[CH:12]=[CH:11][C:9]=2[N:10]=1)(=O)C.[H-].[Na+].[CH:29]1([CH2:32][OH:33])[CH2:31][CH2:30]1>O1CCOCC1>[NH2:4][C:5]1[N:6]=[C:7]([O:33][CH2:32][CH:29]2[CH2:31][CH2:30]2)[C:8]2[N:14]=[C:13]([C:15]3[CH:16]=[CH:17][C:18]([F:21])=[CH:19][CH:20]=3)[CH:12]=[CH:11][C:9]=2[N:10]=1

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 75644CyclopropanemethanolHCID 178474430HCID 178474430, 화합물

생성물 1

HCID 591992052-Amino-4-(cyclopropylmethyloxy)-6-(4-fluorophenyl)pyrido[3,2-d]pyrimidine수율 47%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

To a solution of 2-acetamido-4-(1,2,4-triazolyl)-6-(4-fluorophenyl)-pyrido[3,2-d]pyrimidine (52 mg, 0.15 mmol) in cyclopropylmethanol (1 ml) and dioxane (3 ml) was added NaH (60% dispersion in mineral oil, 0.25 mmol, 15 mg). The reaction mixture was stirred overnight at room temperature. The solvents were evaporated in vacuo, and the residue was purified by preparative TLC, the mobile phase being a methanol/dichloromethane mixture in a ratio of 10:90, yielding the pure title compound (22 mg, yield: 47%) which was characterised as follows: MS (m/z): 311 ([M+H]+, 100).

후처리

  1. customThe solvents were evaporated in vacuo
  2. customthe residue was purified by preparative TLC

출처 및 근거

ORD 기록
ord-95c4a1b41f8146348e4e9172e5d932c9
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08232278B2

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