Dicyclohexylcarbodiimide → HCID 178444548、化合物

HRID 1086971ノート

反応式

HRID 1086971 の反応式
[CH3:1][CH:2]([C:5]1[S:6][C:7]([C:10]2[CH:15]=[CH:14][C:13]([OH:16])=[CH:12][CH:11]=2)=[N:8][N:9]=1)[CH2:3][CH3:4].[CH2:17]([C@H:22]1[CH2:27][CH2:26][C@H:25]([C:28](O)=[O:29])[CH2:24][CH2:23]1)[CH2:18][CH2:19][CH2:20][CH3:21].C1(N=C=NC2CCCCC2)CCCCC1.N1(C2C=CN=CN=2)CCCC1>C(Cl)Cl>[CH3:1][CH:2]([C:5]1[S:6][C:7]([C:10]2[CH:11]=[CH:12][C:13]([O:16][C:28]([C@H:25]3[CH2:26][CH2:27][C@H:22]([CH2:17][CH2:18][CH2:19][CH2:20][CH3:21])[CH2:23][CH2:24]3)=[O:29])=[CH:14][CH:15]=2)=[N:8][N:9]=1)[CH2:3][CH3:4]

参加物

6

反応物 4

HCID 10868DicyclohexylcarbodiimideHCID 218558524-(1-Pyrrolidinyl)pyrimidineHCID 1357784881-Methylpropyl-5-[4-hydroxyphenyl]-1,3,4-thiadiazoleHCID 178444557HCID 178444557、化合物

生成物 1

HCID 178444548HCID 178444548、化合物収率 45.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Into a mixture of 0.3 g (1.28×10-3 mol) of 1-methylpropyl-5-[4-hydroxyphenyl]-1,3,4-thiadiazole, 0.26 g (1.31×10-3 mol) of trans-4-n-pentylcyclohexanecarboxylic acid, 0.27 g (1.31×10-3 mol) of dicyclohexylcarbodiimide and 0.03 g of 4-(1-pyrrolidinyl)pyrimidine, 15 ml of methylene chloride was added, followed by 20 hours of stirring at room temperature. After the reaction, the reaction was filtered and the solid was washed with methylene chloride. The filtrate and the washing liquid were dehydrated, and the solvent was distilled off therefrom to obtain a crude product, which was then recrystallized twice to obtain 0.24 g of 2-(1-methylpropyl)-5-[4-(trans-4-n-pentylcyclohexylcarbonyloxy)-phenyl]-1,3,4-thiadiazole. (Yield: 45.2%).

後処理

  1. additionwas added
  2. customAfter the reaction
  3. filtrationthe reaction was filtered
  4. washthe solid was washed with methylene chloride
  5. distillationthe solvent was distilled off
  6. customto obtain a crude product, which
  7. customwas then recrystallized twice

出典と根拠

ORDレコード
ord-1f6ca3367e6c4a789589b764dd7ea3f3
出典データセット
uspto-grants-1991_07
特許番号
US05034151

反応ノート

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