Hydrochloric Acid → 1-[3-Chloro-5-(trifluoromethyl)pyridin-2-yl]methanamine--hydrogen chloride (1/1)

HRID 897161

反応式

HRID 897161 の反応式
[Cl:1][C:2]1[C:3]([C:12]#[N:13])=[N:4][CH:5]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:7]=1.Cl.[H][H]>[Pd].CO>[ClH:1].[NH2:13][CH2:12][C:3]1[C:2]([Cl:1])=[CH:7][C:6]([C:8]([F:11])([F:10])[F:9])=[CH:5][N:4]=1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14733743-Chloro-5-(trifluoromethyl)pyridine-2-carbonitrileHCID 178418361HCID 178418361、化合物

生成物 1

HCID 114997441-[3-Chloro-5-(trifluoromethyl)pyridin-2-yl]methanamine--hydrogen chloride (1/1)収率 95%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

A mixture of 3-chloro-2-cyano-5-trifluoromethylpyridine (5.1 g) and 5% palladium on charcoal (5.1 mg as Pd metal) was stirred at 20° C. with methanol and concentrated hydrochloric acid (2.5 ml) under 1 atmosphere of hydrogen. After 4 hours the reaction was judged to be complete by hplc. The mixture was filtered through Celatom, washed with methanol and water and evaporated to give 2-aminomethyl-3-chloro-5-trifluoromethylpyridine hydrochloride in 95-97% yield, NMR (in D2O) 4.6 (s, 2H), 8.35 (s, 1H), 8.9 (s, 1H).

後処理

  1. filtrationThe mixture was filtered through Celatom
  2. washwashed with methanol and water
  3. customevaporated

出典と根拠

ORDレコード
ord-192a1acd8be649b0a301875749fc4a39
出典データセット
uspto-grants-2005_07
特許番号
US06921828B2

関連ノート

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