2-Amino-4-chloropyrimidine → HCID 60161632、化合物

HRID 243319

反応式

HRID 243319 の反応式
[C:1]1([N:7]2[C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=3[N:9]=[C:8]2[C@@H:16]([NH2:18])[CH3:17])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl[C:20]1[CH:25]=[CH:24][N:23]=[C:22]([NH2:26])[N:21]=1>C(O)C>[C:1]1([N:7]2[C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=3[N:9]=[C:8]2[C@@H:16]([NH:18][C:20]2[CH:25]=[CH:24][N:23]=[C:22]([NH2:26])[N:21]=2)[CH3:17])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

4

反応物 2

HCID 2233322-Amino-4-chloropyrimidineHCID 68157455(1S)-1-(1-Phenyl-1H-benzimidazol-2-yl)ethan-1-amine

生成物 1

HCID 60161632HCID 60161632、化合物収率 45.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
100 °C

実験手順

Into a 25-mL round-bottom flask was placed a solution of (S)-1-(1-phenyl-1H-benzo[d]imidazol-2-yl)ethanamine from Example 4 (238 mg, 1.00 mmol, 1.00 equiv) in ethanol (8 mL) and 4-chloropyrimidin-2-amine (130 mg, 0.99 mmol, 0.98 equiv, 98%). The resulting solution was stirred overnight at 100° C. and concentrated under vacuum. The crude product was applied onto a C18 Column (water/acetonitrile) to afford 150 mg (44%) of 145 as a white solid. LC-MS (ES, m/z): 331 [M+H]+ H-NMR (300 MHz, CD3OD, ppm): δ 7.83 (d, 1H), 7.57 (m, 8H), 6.11 (q, 1H), 5.61 (q, 1H), 1.67 (d, 3H)

後処理

  1. customInto a 25-mL round-bottom flask was placed
  2. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-38eef9e5d8a54aadabfb54f4e5de317f
出典データセット
uspto-grants-2014_02
特許番号
US08653089B2

関連ノート

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