Hydrochloric Acid → HCID 22011008, 화합물

HRID 323170노트

반응식

HRID 323170 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:9]([C:14]([NH:16][C:17]3[CH:38]=[CH:37][C:20]([C:21]([N:23]([CH2:31][C:32](OCC)=[O:33])[C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=4[CH3:30])=[O:22])=[CH:19][CH:18]=3)=[O:15])=[CH:10][CH:11]=[CH:12][CH:13]=2)=[CH:4][CH:3]=1.[BH4-].[Na+].Cl>C(O)C.C(OCC)(=O)C>[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[C:9]([C:14]([NH:16][C:17]3[CH:18]=[CH:19][C:20]([C:21]([N:23]([CH2:31][CH2:32][OH:33])[C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=4[CH3:30])=[O:22])=[CH:37][CH:38]=3)=[O:15])=[CH:10][CH:11]=[CH:12][CH:13]=2)=[CH:6][CH:7]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 4311764Sodium borohydride2회HCID 22010672HCID 22010672, 화합물

생성물 1

HCID 22011008HCID 22011008, 화합물수율 76.3%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 4-(4′-methylbiphenyl-2-carboxamido)-N-ethoxycarbonylmethyl-N-(2-methylphenyl)benzamide (100 mg) in ethanol (5 ml) was added sodium borohydride (37 mg) at 0° C. and the mixture was stirred for 2 hours at ambient temperature. Since the reaction was not completed and it was so slow, sodium borohydride (220 mg) was added to the mixture at 0° C. and stirred overnight. The reaction mixture was neutralized with 1N hydrochloric acid and diluted with ethyl acetate. The organic layer was washed with brine and dried over magnesium sulfate. Filtering and the removal of solvents afforded 4-(4′-methylbiphenyl-2-carboxamido)-N-(2-hydroxyethyl)-N-(2-methylphenyl)benzamide (70 mg) as a colorless prisms.

후처리

  1. stirringstirred overnight
  2. washThe organic layer was washed with brine
  3. dry with materialdried over magnesium sulfate
  4. filtrationFiltering
  5. customthe removal of solvents

출처 및 근거

ORD 기록
ord-3b67006252cb49ef84005d989d1e1616
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06211242B1

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