Nitric Acid → 5-Chloro-6-nitro-1-indanone

HRID 46630

반응식

HRID 46630 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[C:7](=[O:11])[CH2:6][CH2:5]2.[N+:12]([O-])([OH:14])=[O:13]>>[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[N+:12]([O-:14])=[O:13])[C:7](=[O:11])[CH2:6][CH2:5]2

참가 물질

3

반응물 2

HCID 944Nitric AcidHCID 1425995-Chloro-1-indanone

생성물 1

HCID 221190235-Chloro-6-nitro-1-indanone

반응 조건

온도
-20 °C

실험 절차

86.0 g (0.51 mole) of 5-chloro-1-indanone are introduced in portions into 540 ml of fuming nitric acid (d=1.54), cooled to -20° C., so that the temperature of the reaction mixture remains between -10° and -15° C. After the addition has ended, the mixture is subsequently stirred for 45 minutes at -15° to -20° C., the reaction solution is poured onto ice and the precipitate which has separated out is filtered off and washed with water. The crude product of melting point 110°-113° is recrystallized from ethanol, whereby the melting point of the pure 5-chloro-6-nitro-1-indanone rises to 126°-128° C.

후처리

  1. customremains between -10° and -15° C
  2. additionAfter the addition
  3. additionthe reaction solution is poured onto ice
  4. customthe precipitate which has separated out
  5. filtrationis filtered off
  6. washwashed with water
  7. customThe crude product of melting point 110°-113° is recrystallized from ethanol, whereby the melting point of the pure 5-chloro-6-nitro-1-indanone
  8. customrises to 126°-128° C.

출처 및 근거

ORD 기록
ord-d3a6c63b4a5c415e88d600c12938b6bd
출처 데이터셋
uspto-grants-1979_11
특허 번호
US04174397

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