1-Methylpiperazine → HCID 23035201、化合物

HRID 35561ノート

反応式

HRID 35561 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.[Cl:8][C:9]1[CH:14]=[C:13]([N:15]2[C:20](=[O:21])[NH:19][C:18](=[O:22])[CH:17]=[N:16]2)[CH:12]=[C:11]([Cl:23])[C:10]=1[CH:24]([C:28]1[CH:33]=[CH:32][C:31]([Cl:34])=[CH:30][CH:29]=1)[C:25](Cl)=[O:26]>O1CCCC1>[Cl:34][C:31]1[CH:32]=[CH:33][C:28]([CH:24]([C:10]2[C:9]([Cl:8])=[CH:14][C:13]([N:15]3[C:20](=[O:21])[NH:19][C:18](=[O:22])[CH:17]=[N:16]3)=[CH:12][C:11]=2[Cl:23])[C:25]([N:5]2[CH2:6][CH2:7][N:2]([CH3:1])[CH2:3][CH2:4]2)=[O:26])=[CH:29][CH:30]=1

参加物

4

反応物 2

HCID 531671-MethylpiperazineHCID 225573202,6-dichloro-alpha-(4-chlorophenyl)-4(4,5-dihydro-3,5-dioxo-1,2,4-triazin-2(3H)-yl)benzeneacetylchloride

生成物 1

HCID 23035201HCID 23035201、化合物収率 62.8%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a stirred mixture of 10 parts of 1-methylpiperazine in 45 parts of tetrahydrofuran was added dropwise a solution of 6.7 parts of 2,6-dichloro-α-(4-chlorophenyl)-4-(4,5-dihydro-3,5-dioxo-1,2,4-triazin-2(3H)-yl)benzeneacetyl chloride in 45 parts of tetrahydrofuran during a period of 5 minutes. Upon complete addition, stirring was continued for 2 hours at room temperature. After evaporation in vacuo, the residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (90:10 by volume) as eluent. The pure fractions were collected and the eluent was evaporated in vacuo. The residue was boiled in acetonitrile. After cooling, the precipitated product was filtered off, washed with 2,2'-oxybispropane and dried, yielding 4.8 parts (62.8%) of 1-[2-(4-chlorophenyl)-2-[2,6-dichloro-4-(4,5-dihydro-3,5-dioxo-1,2,4-triazin-2(3H)-yl)phenyl]acetyl]-4-methylpiperazine; mp. 261.5° C. (intermediate 36).

後処理

  1. additionUpon complete addition
  2. customAfter evaporation in vacuo
  3. customthe residue was purified by column chromatography over silica gel using
  4. additiona mixture of trichloromethane and methanol (90:10 by volume) as eluent
  5. customThe pure fractions were collected
  6. customthe eluent was evaporated in vacuo
  7. temperatureAfter cooling
  8. filtrationthe precipitated product was filtered off
  9. washwashed with 2,2'-oxybispropane
  10. customdried

出典と根拠

ORDレコード
ord-e1c86fddfdad44c4888e4de28be5b65c
出典データセット
uspto-grants-1988_08
特許番号
US04767760

反応ノート

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