Piperazine → HCID 68843659、化合物

HRID 1517400ノート

反応式

HRID 1517400 の反応式
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.[C:7]([NH:10][C:11]1[N:12]=[C:13](C2N=CNN=2)[C:14]2[N:20]=[C:19]([C:21]3[CH:26]=[CH:25][C:24]([O:27][CH3:28])=[C:23]([O:29][CH3:30])[CH:22]=3)[CH:18]=[CH:17][C:15]=2[N:16]=1)(=[O:9])[CH3:8]>O1CCOCC1>[C:7]([NH:10][C:11]1[N:12]=[C:13]([N:1]2[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]2)[C:14]2[N:20]=[C:19]([C:21]3[CH:26]=[CH:25][C:24]([O:27][CH3:28])=[C:23]([O:29][CH3:30])[CH:22]=3)[CH:18]=[CH:17][C:15]=2[N:16]=1)(=[O:9])[CH3:8]

参加物

4

反応物 2

HCID 4837PiperazineHCID 178488517HCID 178488517、化合物

生成物 1

HCID 68843659HCID 68843659、化合物収率 79%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

Piperazine (430 mg, 5 mmole) was added to a stirred suspension of 2-acetamido-6-(3,4-dimethoxyphenyl)-4-(1,2,4-triazolyl)pyrido[3,2-d]pyrimidine (977 mg, 2.5 mmole) in dioxane (70 ml). The reaction mixture was refluxed for 16 hours. The precipitate was filtered off and washed with a small amount of dioxane. The filtrate was evaporated to dryness and the residue washed with diethyl ether. Both fractions (the precipitate and the washed filtrate) were combined, resulting in the pure title compound (805 mg, yield 79%) which was characterized by its mass spectrum as follows: MS (m/z): 409 ([M+H]+, 100).

後処理

  1. temperatureThe reaction mixture was refluxed for 16 hours
  2. filtrationThe precipitate was filtered off
  3. washwashed with a small amount of dioxane
  4. customThe filtrate was evaporated to dryness
  5. washthe residue washed with diethyl ether

出典と根拠

ORDレコード
ord-21f6ffaa6cf846318ced0ce1dd2c8f18
出典データセット
uspto-grants-2012_07
特許番号
US08232278B2

反応ノート

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