Hydrochloric Acid → 2-(2',4'-Dichlorophenyl)-5,5-dimethyl-1,3-cyclohexanedione

HRID 65274노트

반응식

HRID 65274 반응식
[Cl:1][C:2]1[CH:7]=[C:6](N)[CH:5]=[CH:4][C:3]=1[CH:9]1[C:14](=[O:15])[CH2:13][C:12]([CH3:17])([CH3:16])[CH2:11][C:10]1=[O:18].[ClH:19].N([O-])=O.[Na+]>O>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:19])[CH:5]=[CH:4][C:3]=1[CH:9]1[C:14](=[O:15])[CH2:13][C:12]([CH3:17])([CH3:16])[CH2:11][C:10]1=[O:18]

참가 물질

5

반응물 3

HCID 313Hydrochloric Acid2회HCID 128765962-(2'-Chloro-4'-aminophenyl)-5,5-dimethyl-1,3-cyclohexanedioneHCID 23668193Sodium Nitrite2회

생성물 1

HCID 128766202-(2',4'-Dichlorophenyl)-5,5-dimethyl-1,3-cyclohexanedione

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
10 °C

실험 절차

A suspension of 5.00 g (0.0188 mol) of 2-(2'-chloro-4'-aminophenyl)-5,5-dimethyl-1,3-cyclohexanedione in 75 ml of water containing 4.0 ml of concentrated HCl was stirred and heated almost to boiling for 10 min., then cooled to 10° C. and an additional 7 ml of conc. HCl added and the solution cooled to 0°-5° C. A solution of 2.00 g (0.0282 mol) of sodium nitrite in 6.0 ml of water was added dropwise to the amine hydrochloride solution while maintaining the temperature at 0°-5° C. When all the NaNO2 solution had been added, the diazonium salt solution was stirred for 30 min. at 0° C.

후처리

  1. temperatureheated almost
  2. temperaturethe solution cooled to 0°-5° C
  3. temperaturewhile maintaining the temperature at 0°-5° C

출처 및 근거

ORD 기록
ord-571b0fafc8de43bcab3f69070ebbba20
출처 데이터셋
uspto-grants-1986_09
특허 번호
US04613617

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