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

HRID 2379190ノート

反応式

HRID 2379190 の反応式
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]

参加物

4

反応物 2

HCID 4311764Sodium borohydrideHCID 18958065HCID 18958065、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-36d75a62a53042c990fbac768beb8bc6
出典データセット
uspto-grants-1994_11
特許番号
US05360822

反応ノート

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