Cyclopentylamine → HCID 11219722、化合物

HRID 969742ノート

反応式

HRID 969742 の反応式
[CH:1]1([NH2:6])[CH2:5][CH2:4][CH2:3][CH2:2]1.C(N(CC)CC)C.[Cl:14][C:15]1[C:20]([CH:21]([CH3:23])[CH3:22])=[C:19](Cl)[N:18]2[N:25]=[CH:26][N:27]=[C:17]2[N:16]=1>C(Cl)Cl>[Cl:14][C:15]1[C:20]([CH:21]([CH3:22])[CH3:23])=[C:19]([NH:6][CH:1]2[CH2:5][CH2:4][CH2:3][CH2:2]2)[N:18]2[N:25]=[CH:26][N:27]=[C:17]2[N:16]=1

参加物

5

反応物 3

HCID 2906CyclopentylamineHCID 8471TriethylamineHCID 11345254[1,2,4]Triazolo[1,5-a]pyrimidine, 5,7-dichloro-6-(1-methylethyl)-

生成物 1

HCID 11219722HCID 11219722、化合物収率 76%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

With stirring, a mixture of 0.13 g (1.5 mmol) of cyclopentylamine and 0.15 g (1.5 mmol) of triethylamine in 10 ml of methylene chloride was added to a mixture of 0.34 g (1.5 mmol) of 5,7-dichloro-6-isopropyl-[1,2,4]-triazolo-[1,5-α]-pyrimidine (cf. Ex. 2) in 20 ml of methylene chloride. The reaction mixture was stirred at room temperature for 16 h and then washed with 5% strength hydrochloric acid. The organic phase was separated off, dried over sodium sulfate and filtered. The filtrate was freed from the solvent and the residue was purified chromatographically. This gave 0.32 g (1.14 mmol) of the title compound (melting point 139° C.).

後処理

  1. stirringThe reaction mixture was stirred at room temperature for 16 h
  2. washwashed with 5% strength hydrochloric acid
  3. customThe organic phase was separated off
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. customthe residue was purified chromatographically

出典と根拠

ORDレコード
ord-123f145a17f94a23b7aadd091ac54852
出典データセット
uspto-grants-2007_12
特許番号
US07307172B2

反応ノート

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