Sodium borohydride → HCID 14990561, 화합물

HRID 2166032노트

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HRID 2166032 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:10]2[CH:21]=[CH:20][C:13]3[N:14]([CH:17]([CH3:19])[CH3:18])[N:15]=[N:16][C:12]=3[CH:11]=2)=[O:9])=[CH:4][CH:3]=1.[BH4-].[Na+]>C(O)C>[F:1][C:2]1[CH:3]=[CH:4][C:5]([CH:8]([C:10]2[CH:21]=[CH:20][C:13]3[N:14]([CH:17]([CH3:18])[CH3:19])[N:15]=[N:16][C:12]=3[CH:11]=2)[OH:9])=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 4311764Sodium borohydrideHCID 14990560HCID 14990560, 화합물

생성물 1

HCID 14990561HCID 14990561, 화합물수율 62.5%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a stirred solution of 17 parts of (4-fluorophenyl) [1-(1-methylethyl)-1H-benzotriazol-5-yl]methanone in 80 parts of ethanol were added 3.4 parts of sodium tetrahydroborate. After stirring for 1 hour at room temperature, the reaction mixture was neutralized to pH 7. The reaction mixture was concentrated and the product was extracted with ethyl acetate. The extract was dried, filtered and evaporated. The residue was purified by column chromatography over silica gel using a mixture of dichloromethane and methanol (98:2 by volume) as eluent. The pure fractions were collected and the eluent was evaporated, yielding 10.7 parts (62.5%) of α-(4-fluorophenyl)-1-(1-methylethyl)-1H-benzotriazole-5-methanol as a residue (int. 4).

후처리

  1. concentrationThe reaction mixture was concentrated
  2. extractionthe product was extracted with ethyl acetate
  3. customThe extract was dried
  4. filtrationfiltered
  5. customevaporated
  6. customThe residue was purified by column chromatography over silica gel using
  7. additiona mixture of dichloromethane and methanol (98:2 by volume) as eluent
  8. customThe pure fractions were collected
  9. customthe eluent was evaporated

출처 및 근거

ORD 기록
ord-488be89842b74e2db449cbbae8f9921f
출처 데이터셋
uspto-grants-1990_07
특허 번호
US04943574

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