Formaldehyde → HCID 23300015、化合物

HRID 1952747

反応式

HRID 1952747 の反応式
[O:1]1[C:6]2[CH:7]=[CH:8][CH:9]=[C:10]([N:11]3[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]3)[C:5]=2[O:4][CH2:3][CH2:2]1.[CH2:17]=O.[NH2:19][C:20]1[CH:24]=[C:23]([NH2:25])[N:22]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[N:21]=1>>[NH2:19][C:20]1[C:24]([CH2:17][N:14]2[CH2:15][CH2:16][N:11]([C:10]3[C:5]4[O:4][CH2:3][CH2:2][O:1][C:6]=4[CH:7]=[CH:8][CH:9]=3)[CH2:12][CH2:13]2)=[C:23]([NH2:25])[N:22]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[N:21]=1

参加物

4

反応物 3

HCID 712FormaldehydeHCID 65853EltoprazineHCID 233000651-Phenyl-1H-pyrazole-3,5-diamine

生成物 1

HCID 23300015HCID 23300015、化合物

実験手順

A mixture of 1-(1,4-benzodioxan-5-yl)piperazine (0.8 g; prepared in a similar manner to that described in Example 2), 37-40% aqueous formaldehyde solution (0.27 ml) and industrial methylated spirit (10 ml) was stirred at ambient temperature under nitrogen for 18 hours, then a solution of 3,5-diamino-1-phenylpyrazole (0.63 g) in industrial methylated spirit (8 ml) was added dropwise. The mixture was stirred at ambient temperature for 2.5 hours, then the solvent was removed in vacuo, and the residue was purified by flash chromatography over silica using an approximately 9:1 mixture of dichloromethane and methanol as eluant. Appropriate fractions were combined and the solvents removed in vacuo to leave 3,5-diamino-4-[4-(1,4-benzodioxan-5-yl)piperazin-1-ylmethyl]-1-phenylpyrazole as a pale pink solid (0.38 g), m.p. 84-87° C.

後処理

  1. customprepared in a similar manner to that
  2. stirringThe mixture was stirred at ambient temperature for 2.5 hours
  3. customthe solvent was removed in vacuo
  4. customthe residue was purified by flash chromatography over silica using
  5. additionan approximately 9:1 mixture of dichloromethane and methanol as eluant
  6. customthe solvents removed in vacuo

出典と根拠

ORDレコード
ord-bd722e59947e452da3d25ac68af1822d
出典データセット
uspto-grants-2000_09
特許番号
US06114334

関連ノート

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