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

HRID 1517434ノート

反応式

HRID 1517434 の反応式
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

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 75644CyclopropanemethanolHCID 178474430HCID 178474430、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-95c4a1b41f8146348e4e9172e5d932c9
出典データセット
uspto-grants-2012_07
特許番号
US08232278B2

反応ノート

読み込み中…