Sodium hydride → HCID 178462378、化合物

HRID 60531ノート

反応式

HRID 60531 の反応式
[H-].[Na+].[BH4-].[Na+].O.[NH2:6][C:7]1[N:12]=[C:11]([SH:13])[N:10]=[C:9]([OH:14])[CH:8]=1.Cl[C@@H:16]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[CH3:17]>CN(C=O)C>[NH2:6][C:7]1[N:12]=[C:11]([S:13][C@H:16]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH3:17])[N:10]=[C:9]([OH:14])[CH:8]=1

参加物

6

反応物 4

HCID 24758Sodium hydrideHCID 642190((1R)-1-Chloroethyl)benzeneHCID 4311764Sodium borohydrideHCID 178507962HCID 178507962、化合物

生成物 1

HCID 178462378HCID 178462378、化合物収率 46.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

NaH (60% in oil) (0.5 g, 12.5 mmol) followed by NaBH4 (40 mg, 1 mmol) was added to 6-amino-2-mercaptopyrimidin-4-ol monohydrate (1.6 g, 10 mmol) in DMF (20 mL). After 30 min, [(1R)-1-chloroethyl]benzene (1.4 g, 10 mmol) was added and the reaction mixture was stirred for 16 h. The reaction was concentrated in vacuo to ca. 10 mL volume and then poured into water (ca. 50 mL). The precipitated solid material was filtered off and washed with water and ether to give the title compound (1.15 g, 46% yield).

後処理

  1. concentrationThe reaction was concentrated in vacuo to ca. 10 mL volume
  2. additionpoured into water (ca. 50 mL)
  3. filtrationThe precipitated solid material was filtered off
  4. washwashed with water and ether

出典と根拠

ORDレコード
ord-fe4087e49a5f4d0798cd54d0f8e0d74f
出典データセット
uspto-grants-2016_09
特許番号
US09440992B2

反応ノート

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