Hydrochloric Acid → 2-(3-Bromo-5-methoxyphenyl)ethan-1-amine

HRID 2069079ノート

反応式

HRID 2069079 の反応式
C1COCC1.[Br:6][C:7]1[CH:8]=[C:9]([CH2:15][C:16]#[N:17])[CH:10]=[C:11]([O:13][CH3:14])[CH:12]=1.Cl.[OH-].[Na+]>C(OCC)(=O)C.CO>[Br:6][C:7]1[CH:8]=[C:9]([CH2:15][CH2:16][NH2:17])[CH:10]=[C:11]([O:13][CH3:14])[CH:12]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 212429652-(3-Bromo-5-methoxyphenyl)acetonitrile

生成物 1

HCID 106094762-(3-Bromo-5-methoxyphenyl)ethan-1-amine

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
80 °C

実験手順

A borane-tetrahydrofuran complex (1 M, 73.6 mL) was added to a THF (36.8 mL) solution of Intermediate 3 at room temperature and the resulting mixture was stirred to reflux at 80° C. for 2 hours. Methanol (26 mL) and 1 N hydrochloric acid (26 mL) were added to the reaction mixture solution and the resulting mixture was stirred at room temperature for 1 hour. The resulting mixture was neutralized with 1 N aqueous sodium hydroxide solution followed by the addition of ethyl acetate (100 mL) to extract the reaction mixture, the organic layer was dried, and then the solvent was evaporated under reduced pressure to give the title compound (8.76 g).

後処理

  1. stirringthe resulting mixture was stirred at room temperature for 1 hour
  2. extractionto extract the reaction mixture
  3. customthe organic layer was dried
  4. customthe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-311631ca28cd4032830eee9f6352f8bd
出典データセット
uspto-grants-2012_10
特許番号
US08299055B2

反応ノート

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