Hydrochloric Acid → HCID 90020647、化合物

HRID 2200141ノート

反応式

HRID 2200141 の反応式
[BH4-].[Na+].[N+:3]([C:6]1[CH:7]=[C:8]([C:16](=[O:18])[CH3:17])[CH:9]=[C:10]([C:12]([F:15])([F:14])[F:13])[CH:11]=1)([O-:5])=[O:4].Cl>CO>[N+:3]([C:6]1[CH:7]=[C:8]([CH:16]([OH:18])[CH3:17])[CH:9]=[C:10]([C:12]([F:13])([F:14])[F:15])[CH:11]=1)([O-:5])=[O:4]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 4311764Sodium borohydrideHCID 534027751-[3-Nitro-5-(trifluoromethyl)phenyl]ethanone

生成物 1

HCID 90020647HCID 90020647、化合物収率 91.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Add sodium borohydride (95 mg, 2.44 mmol) to a solution of 1-(3-nitro-5-(trifluoromethyl)phenyl)ethanone (570 mg, 2.44 mmol) in methanol (5 mL), stir the mixture for 15 min at ambient temperature. Quench the reaction with water, adjust pH=7 with 1N hydrochloric acid, extract with ethyl acetate (50 mL×3), combine the organic layers, wash with brine, dry over sodium sulfate. Concentrate under reduced pressure to provide the crude product. Purify by flash chromatography (silica gel, EtOAc:PE=1:10) to afford the title compound (520 mg, 91.2%).

後処理

  1. customQuench
  2. customthe reaction with water
  3. extractionextract with ethyl acetate (50 mL×3)
  4. washwash with brine
  5. dry with materialdry over sodium sulfate
  6. concentrationConcentrate under reduced pressure
  7. customto provide the crude product
  8. customPurify by flash chromatography (silica gel, EtOAc:PE=1:10)

出典と根拠

ORDレコード
ord-d1fb88e606eb41778be31f98c05b9c4d
出典データセット
uspto-grants-2016_06
特許番号
US09359338B2

反応ノート

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