Oxalic Acid → HCID 178526031、化合物

HRID 486053

反応式

HRID 486053 の反応式
[CH2:1]([N:9]=[C:10]=[S:11])[CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[NH:12]1[CH:16]=[C:15]([CH:17]2[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]2)[N:14]=[CH:13]1.[C:23]([OH:28])(=[O:27])[C:24]([OH:26])=[O:25]>C1(C)C=CC=CC=1.C(O)(C)C>[C:23]([OH:28])(=[O:27])[C:24]([OH:26])=[O:25].[CH2:1]([NH:9][C:10]([N:20]1[CH2:19][CH2:18][CH:17]([C:15]2[N:14]=[CH:13][NH:12][CH:16]=2)[CH2:22][CH2:21]1)=[S:11])[CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1

参加物

6

反応物 3

HCID 971Oxalic AcidHCID 16741Phenethyl IsothiocyanateHCID 1784208734-(1H-imidazol-4-yl)piperidine

生成物 1

HCID 178526031HCID 178526031、化合物

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 3776Isopropanol溶媒

反応条件

温度
80 °C

実験手順

A solution of 1.63 g (0.01 mol) of phenethyl isothiocyanate in 60 ml of toluene and 1.51 g (0.01 mol) of 4-(4-imidazolyl)piperidine is heated to reflux for 1h 30 min. After cooling, the solution is evaporated under reduced pressure and the residual oil obtained is dissolved in 60 ml of isopropanol in the presence of 1.2 equivalents of oxalic acid. After 30 minutes of heating at 80° C., the white precipitate formed is drained, washed with ether and recrystallised in acetonitrile.

後処理

  1. temperatureAfter cooling
  2. customthe solution is evaporated under reduced pressure
  3. customthe residual oil obtained
  4. customthe white precipitate formed
  5. washwashed with ether
  6. customrecrystallised in acetonitrile

出典と根拠

ORDレコード
ord-474f4c34d56c412e9d2b44ede976dcb9
出典データセット
uspto-grants-1994_03
特許番号
US05290790

関連ノート

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