Sodium borohydride → N-[3-(2-Amino-1-hydroxyethyl)-4-fluorophenyl]methanesulfonamide

HRID 2379190노트

반응식

HRID 2379190 반응식
Cl.[NH2:2][CH2:3][C:4]([C:6]1[CH:7]=[C:8]([CH:14]=[CH:15][C:16]=1[F:17])[NH:9][S:10]([CH3:13])(=[O:12])=[O:11])=[O:5].[BH4-].[Na+]>CO>[NH2:2][CH2:3][CH:4]([C:6]1[CH:7]=[C:8]([CH:14]=[CH:15][C:16]=1[F:17])[NH:9][S:10]([CH3:13])(=[O:11])=[O:12])[OH:5]

참가 물질

4

반응물 2

HCID 4311764Sodium borohydrideHCID 18958065HCID 18958065, 화합물

생성물 1

HCID 9838761N-[3-(2-Amino-1-hydroxyethyl)-4-fluorophenyl]methanesulfonamide수율 91.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

3'-(2-Aminoacetyl)-4'-fluoromethanesulfonanilide hydrochloride (3 g) was dissolved in 30 ml of methanol, 0.20 g of sodium borohydride was added at 0°-5° C. and the mixture was made to react at the same temperature for 1 hour. The solvent was evaporated and the residue was made into free base using ion exchange resin (Dowex 50W X2), concentrated to dryness and the residue was recrystallized from methanol to give 2.4 g of (±)-3'-(2-amino-1-hydroxyethyl)-4'-fluoromethanesulfonanilide, m.p. 176°-179° C.

후처리

  1. customto react at the same temperature for 1 hour
  2. customThe solvent was evaporated
  3. concentrationconcentrated to dryness
  4. customthe residue was recrystallized from methanol

출처 및 근거

ORD 기록
ord-36d75a62a53042c990fbac768beb8bc6
출처 데이터셋
uspto-grants-1994_11
특허 번호
US05360822

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