Dicyclohexylcarbodiimide → HCID 178418537、化合物

HRID 4162

反応式

HRID 4162 の反応式
[C:1]([C:4]1[CH:5]=[C:6]([N:10]2[C:14]([SH:15])=[N:13][N:12]=[N:11]2)[CH:7]=[CH:8][CH:9]=1)([OH:3])=O.[CH:16]([NH:18][NH:19][C:20]1[CH:26]=[CH:25][C:23]([NH2:24])=[CH:22][CH:21]=1)=[O:17].C1(N=C=NC2CCCCC2)CCCCC1>CN(C)C=O>[SH:15][C:14]1[N:10]([C:6]2[CH:7]=[CH:8][CH:9]=[C:4]([C:1](=[O:3])[NH:24][C:23]3[CH:22]=[CH:21][C:20]([NH:19][NH:18][CH:16]=[O:17])=[CH:26][CH:25]=3)[CH:5]=2)[N:11]=[N:12][N:13]=1

参加物

5

反応物 3

HCID 10868DicyclohexylcarbodiimideHCID 113189Hydrazinecarboxaldehyde, 2-(4-aminophenyl)-HCID 178418535HCID 178418535、化合物

生成物 1

HCID 178418537HCID 178418537、化合物収率 25.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

In 50 ml of dimethylformamide were dissolved 11.1 g of 1-(3-carboxyphenyl)-5-mercaptotetrazole and 7.6 g of 4-(2-formylhydrazino)aniline, and a solution of 10.3 g of dicyclohexylcarbodiimide in 10 ml of dimethylformamide was added dropwise to the solution at 0° C. in a nitrogeneous atmosphere over about 30 minutes. After the addition, the mixture was stirred at room temperature for 3 hours. The precipitated dicyclohexylurea was separated by filtration, and the filtrate was added to 500 ml of ice-water while stirring. The thus precipitated crystals were filtered, washed with water and dispersed in 100 ml of hot methanol. The dispersion was allowed to cool to room temperature and filtered. The filtrate was washed with methanol to obtain 4.5 g of the desired compound. Melting point: 202° C. (with decomposition).

後処理

  1. additionAfter the addition
  2. customThe precipitated dicyclohexylurea was separated by filtration
  3. additionthe filtrate was added to 500 ml of ice-water
  4. stirringwhile stirring
  5. filtrationThe thus precipitated crystals were filtered
  6. washwashed with water
  7. additiondispersed in 100 ml of hot methanol
  8. temperatureto cool to room temperature
  9. filtrationfiltered
  10. washThe filtrate was washed with methanol

出典と根拠

ORDレコード
ord-91b5da6b753c4d87a85d7b0c1e08baeb
出典データセット
uspto-grants-1988_02
特許番号
US04724199

関連ノート

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