Imidazole → HCID 20286585, 화합물

HRID 126879

반응식

HRID 126879 반응식
Br[CH:2]([O:10][C:11]1[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][CH:12]=1)[C:3](=[O:9])[C:4]([CH3:8])([CH3:7])[CH2:5][Cl:6].[NH:18]1[CH:22]=[CH:21][N:20]=[CH:19]1.[C:23]1([S:37]([OH:40])(=[O:39])=[O:38])[C:32]2[CH:31]=[CH:30][CH:29]=[C:28]([S:33]([OH:36])(=[O:35])=[O:34])[C:27]=2[CH:26]=[CH:25][CH:24]=1>C(#N)C.CC(C)=O>[C:23]1([S:37]([OH:40])(=[O:39])=[O:38])[C:32]2[CH:31]=[CH:30][CH:29]=[C:28]([S:33]([OH:36])(=[O:35])=[O:34])[C:27]=2[CH:26]=[CH:25][CH:24]=1.[Cl:17][C:14]1[CH:15]=[CH:16][C:11]([O:10][CH:2]([N:18]2[CH:22]=[CH:21][N:20]=[CH:19]2)[C:3](=[O:9])[C:4]([CH3:8])([CH3:7])[CH2:5][Cl:6])=[CH:12][CH:13]=1

참가 물질

6

반응물 3

HCID 795ImidazoleHCID 66661,5-Naphthalenedisulfonic acidHCID 20286562HCID 20286562, 화합물

생성물 1

HCID 20286585HCID 20286585, 화합물수율 84.7%

시약·촉매·용매 2

HCID 180Acetone용매HCID 6342Acetonitrile용매

실험 절차

17 g (0.05 mol) of crude 1-bromo-1-(4-chlorophenoxy)-3,3-dimethyl-4-chloro-butan-2-one were dissolved in 100 ml of absolute acetonitrile. 12 g (0.175 mol) of imidazole were added to this solution and the mixture was heated under reflux for 40 hours. Thereafter, it was concentrated by distilling off the solvent in vacuo and the residue was taken up in 300 ml of methylene chloride. The methylene chloride mixture was washed three times with 100 ml of water each time, dried over sodium sulphate and concentrated again in vacuo. The residue was taken up in 100 ml of acetone, and a solution of 9 g (0.038 mol) of 1,5-naphthalenedisulphonic acid in 50 ml of acetone was added. After 2 hours, the precipitate which had formed was filtered off and dried. 19.8 g (80.7% of theory) of 1-(4-chlorophenoxy)-1-(imidazol-1-yl)-3,3-dimethyl-4-chloro-butan-2-one naphthalene-1,5-disulphonate of melting point 266°- 267° C. were obtained. ##STR14##

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 40 hours
  3. concentrationThereafter, it was concentrated
  4. distillationby distilling off the solvent in vacuo
  5. washThe methylene chloride mixture was washed three times with 100 ml of water each time
  6. dry with materialdried over sodium sulphate
  7. concentrationconcentrated again in vacuo
  8. customthe precipitate which had formed
  9. filtrationwas filtered off
  10. customdried

출처 및 근거

ORD 기록
ord-e16aee086878472a9e58aad7c5ba34c4
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04254132

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