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

HRID 704566

반응식

HRID 704566 반응식
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

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 962Water용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-eb0648a2166841f8bb65d587ff7953ac
출처 데이터셋
uspto-grants-1991_01
특허 번호
US04988695

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