Water → HCID 13193051, 화합물

HRID 371251노트

반응식

HRID 371251 반응식
[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]

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 246232,2,3-TrichloropropionaldehydeHCID 12760574HCID 12760574, 화합물

생성물 1

HCID 13193051HCID 13193051, 화합물수율 30.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-aca94391de4b4fff8248eb8d8c6eaaed
출처 데이터셋
uspto-grants-1985_07
특허 번호
US04530715

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