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Water → HCID 22761227, 화합물

HRID 1703440
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HRID 1703440 반응식
[C:1]([NH:9][CH:10]([N:17]1[CH:21]=[CH:20][N:19]=[CH:18]1)[C:11](=[O:16])[C:12]([CH3:15])([CH3:14])[CH3:13])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[BH4-].[Na+].O>CO>[C:1]([NH:9][CH:10]([N:17]1[CH:21]=[CH:20][N:19]=[CH:18]1)[CH:11]([OH:16])[C:12]([CH3:15])([CH3:14])[CH3:13])(=[O:8])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

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HCID 962WaterHCID 4311764Sodium borohydrideHCID 22761232N-(1-(1H-Imidazol-1-yl)-3,3-dimethyl-2-oxobutyl)benzamide

생성물 1

HCID 22761227HCID 22761227, 화합물수율 79%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Process variant (b) 28.5 g (0.1 mol) of 1-benzamido-3,3-dimethyl-1-(imidazol-1-yl)-butan-2-one of melting point 140°-142° C. (prepared analogously to Example 8, in accordance with process (a)) were dissolved in 250 ml of methanol. 4 g (0.1 mol) of sodium borohydride were added in portions while stirring and cooling at 0° to 10° C. Stirring was continued for 15 hours at room temperature and 200 ml of water were added to the reaction mixture. The mixture was then extracted by shaking with 200 ml of methylene chloride and the organic phase as dried over sodium sulphate and concentrated by distilling off the solvent in vacuo. Boiling up with petroleum ether and a little ether caused the mixture to crystallize. 22.6 g (79% of theory) of 1-benzamido-3,3-dimethyl-1-imidazol-1-yl-butan-2-ol of melting point 143° C. were obtained.

후처리

  1. temperaturecooling at 0° to 10° C
  2. stirringStirring
  3. extractionThe mixture was then extracted
  4. stirringby shaking with 200 ml of methylene chloride
  5. dry with materialthe organic phase as dried over sodium sulphate
  6. concentrationconcentrated
  7. distillationby distilling off the solvent in vacuo
  8. customto crystallize

출처 및 근거

ORD 기록
ord-255d753c54d94180ab816e18f65ef0cb
출처 데이터셋
uspto-grants-1978_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04124369

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