Hydrochloric Acid → N-(3-(aminomethyl)-5-isopropylphenyl)acetamide

HRID 2071037ノート

反応式

HRID 2071037 の反応式
[C:1]([C:3]1[CH:4]=[C:5]([NH:12][C:13](=[O:15])[CH3:14])[CH:6]=[C:7]([C:9]([CH3:11])=[CH2:10])[CH:8]=1)#[N:2].[BH4-].[Na+].Cl>CCO>[NH2:2][CH2:1][C:3]1[CH:4]=[C:5]([NH:12][C:13](=[O:15])[CH3:14])[CH:6]=[C:7]([CH:9]([CH3:11])[CH3:10])[CH:8]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 4311764Sodium borohydrideHCID 68669811HCID 68669811、化合物

生成物 1

HCID 59569807N-(3-(aminomethyl)-5-isopropylphenyl)acetamide

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a stirring solution of 91.9 mg (0.459 mmol) of N-(3-cyano-5-(prop-1-en-2-yl)phenyl)acetamide and 110 mg (0.466 mmol) of CoCl2.6H2O in 3 mL of EtOH at 50° C. was added 118 mg of NaBH4 in 2 portions. After 3 h 45 min., 5 N HCl was added to a pH=1, and the mixture was concentrated. Ammonium hydroxide was added to a pH=9, and H2O was also added. The aqueous layer was extracted with the extract of (40 mL CHCl3: 5 mL of MeOH: 5 mL of H2O) (2×). The combined extracts were dried over Na2SO4, filtered, and concentrated to provide the crude N-(3-(aminomethyl)-5-isopropylphenyl)acetamide which was used without further purification.

後処理

  1. concentrationthe mixture was concentrated
  2. additionAmmonium hydroxide was added to a pH=9, and H2O
  3. additionwas also added
  4. extractionThe aqueous layer was extracted with the
  5. extractionextract of (40 mL CHCl3: 5 mL of MeOH: 5 mL of H2O) (2×)
  6. dry with materialThe combined extracts were dried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-464417e3069b4d969c411529081c76f4
出典データセット
uspto-grants-2012_10
特許番号
US08299267B2

反応ノート

読み込み中…