3-(2,4-dichlorophenyl)-3-hydroxy-4-(1H-1,2,4-triazol-1-yl)butyrimidic acid, ethyl ester dihydrochloride → 1-Carbamoyl-2-(2,4-dichlorophenyl)-3-(1H-1,2,4-triazol-1-yl)propan-2-ol

HRID 728330ノート

反応式

HRID 728330 の反応式
Cl.Cl.[Cl:3][C:4]1[CH:9]=[C:8]([Cl:10])[CH:7]=[CH:6][C:5]=1[C:11]([OH:24])([CH2:18][N:19]1[CH:23]=[N:22][CH:21]=[N:20]1)[CH2:12][C:13](=[NH:17])[O:14]CC>ClC1C=CC=CC=1Cl>[C:13]([CH2:12][C:11]([C:5]1[CH:6]=[CH:7][C:8]([Cl:10])=[CH:9][C:4]=1[Cl:3])([OH:24])[CH2:18][N:19]1[CH:23]=[N:22][CH:21]=[N:20]1)(=[O:14])[NH2:17]

参加物

3

反応物 1

HCID 1317139683-(2,4-dichlorophenyl)-3-hydroxy-4-(1H-1,2,4-triazol-1-yl)butyrimidic acid, ethyl ester dihydrochloride

生成物 1

HCID 136030731-Carbamoyl-2-(2,4-dichlorophenyl)-3-(1H-1,2,4-triazol-1-yl)propan-2-ol

試薬・触媒・溶媒 1

HCID 72391,2-Dichlorobenzene溶媒

反応条件

温度
178 °C

実験手順

3-(2,4-Dichlorophenyl)-3-hydroxy-4-(1H-1,2,4-triazol-1-yl)butyrimidic acid, ethyl ester dihydrochloride (3.42 g) was suspended in 1,2-dichlorobenzene (35 ml) and the mixture was heated to the reflux temperature of the solvent [178° C.). After refluxing for five minutes, a solution was obtained. Refluxing was then continued for an additional 10 minutes. The reaction mixture was cooled, evaporated, and the resulting gum was triturated with hexane and heated with acetone. On cooling a cream-colored granular solid was formed which was filtered to yield the title compound as a solvate (1.26 g). On standing overnight in a refrigerator some further solvated product precipitated (0.62 g). After drying at 80° C. for 6 hours to remove the solvent the pure (unsolvated) title compound was obtained, yield 1.5 g, m.p. 144°-145° C.

後処理

  1. temperatureAfter refluxing for five minutes
  2. customa solution was obtained
  3. temperatureRefluxing
  4. temperatureThe reaction mixture was cooled
  5. customevaporated
  6. customthe resulting gum was triturated with hexane
  7. temperatureheated with acetone
  8. temperatureOn cooling a cream-colored granular solid
  9. customwas formed which
  10. filtrationwas filtered

出典と根拠

ORDレコード
ord-5171067bab904d9589ba61d15c4e7183
出典データセット
uspto-grants-1991_09
特許番号
US05047548

反応ノート

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