Water → HCID 13193051、化合物

HRID 371251ノート

反応式

HRID 371251 の反応式
[Cl:1][C:2]([Cl:7])([CH2:5][Cl:6])[CH:3]=[O:4].[CH3:8][C:9]1([C:12](=[O:19])[CH2:13][N:14]2[CH:18]=[N:17][CH:16]=[N:15]2)[CH2:11][CH2:10]1.C(=O)([O-])[O-].[K+].[K+].O>O1CCCC1>[Cl:6][CH2:5][C:2]([Cl:7])([Cl:1])[CH:3]([OH:4])[CH:13]([N:14]1[CH:18]=[N:17][CH:16]=[N:15]1)[C:12]([C:9]1([CH3:8])[CH2:10][CH2:11]1)=[O:19]

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 246232,2,3-TrichloropropionaldehydeHCID 12760574HCID 12760574、化合物

生成物 1

HCID 13193051HCID 13193051、化合物収率 30.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

11.3 g of 2,2,3-trichloropropionaldehyde were added dropwise to 9.2 g (0.056 mol) of 1-methyl-1-(1,2,4-triazol-1-yl-acetyl)-cyclopropane in 120 ml of tetrahydrofuran and 13.6 g (0.1 mol) of potassium carbonate, the temperature increasing slightly. The reaction solution was stirred overnight at room temperature and was thereafter introduced into 500 ml of water. The resulting precipitate was filtered off under suction and recrystallized from methanol. 5.5 g (30% of theory) of 1,2,2-trichloro-3-hydroxy-4-(1,2,4-triazol-1-yl)-5-(1-methylcycloprop-1-yl)-pentan-5-one of melting point 182° to 186° C. were obtained.

後処理

  1. temperaturethe temperature increasing slightly
  2. filtrationThe resulting precipitate was filtered off under suction
  3. customrecrystallized from methanol

出典と根拠

ORDレコード
ord-aca94391de4b4fff8248eb8d8c6eaaed
出典データセット
uspto-grants-1985_07
特許番号
US04530715

反応ノート

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