1-(o-Aminophenyl)-4-chloro-1-butanone hydrochloride → 3-(2-Chloroethyl)-4-oxo-(1H)-cinnoline

HRID 704566ノート

反応式

HRID 704566 の反応式
Cl.[NH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9](=[O:14])[CH2:10][CH2:11][CH2:12][Cl:13].[N:15]([O-])=O.[Na+]>Cl.O>[Cl:13][CH2:12][CH2:11][C:10]1[C:9](=[O:14])[C:4]2[C:3](=[CH:8][CH:7]=[CH:6][CH:5]=2)[NH:2][N:15]=1

参加物

5

反応物 2

HCID 232932461-(o-Aminophenyl)-4-chloro-1-butanone hydrochlorideHCID 23668193Sodium Nitrite

生成物 1

HCID 200727583-(2-Chloroethyl)-4-oxo-(1H)-cinnoline

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 962Water溶媒

実験手順

A solution of 1-(2-aminophenyl)-4-chlorobutan-1-one hydrochloride (b 11.3 g, 0.0427 mol) in concentrated hydrochloric acid (1200 ml) was cooled down to 0° with stirring. Then sodium nitrite (3.54 g, 0.051mol) in water (25 ml) was added dropwise. On completion of the addition, the reaction mixture was allowed to warm to room temperature and stirred overnight. The solution was evaporated under reduced pressure to dryness. The solid obtained was washed with a solution of sodium acetate and collected by filtration to give the title compound, 5.32 g. Recrystallization from methanol gave the product, m.p. 201-203°.

後処理

  1. additionOn completion of the addition
  2. stirringstirred overnight
  3. customThe solution was evaporated under reduced pressure to dryness
  4. customThe solid obtained
  5. washwas washed with a solution of sodium acetate
  6. filtrationcollected by filtration

出典と根拠

ORDレコード
ord-eb0648a2166841f8bb65d587ff7953ac
出典データセット
uspto-grants-1991_01
特許番号
US04988695

反応ノート

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