3-Chlorobenzoic Acid → 3-Chlorobenzoic Acid

HRID 1379249

반응식

HRID 1379249 반응식
[CH:1]1([CH2:8][CH2:9][C:10]#[N:11])[CH2:6][CH2:5][CH2:4][CH2:3][C:2]1=[O:7].ClC1C=CC=C(C(OO)=[O:20])C=1.[Cl:23][C:24]1[CH:25]=[C:26]([CH:30]=[CH:31][CH:32]=1)[C:27]([OH:29])=[O:28]>CCCCCC>[C:10]([CH2:9][CH2:8][CH:1]1[O:20][C:2](=[O:7])[CH2:3][CH2:4][CH2:5][CH2:6]1)#[N:11].[Cl:23][C:24]1[CH:25]=[C:26]([CH:30]=[CH:31][CH:32]=1)[C:27]([OH:29])=[O:28]

참가 물질

6

반응물 3

HCID 4473-Chlorobenzoic AcidHCID 70297m-Chloroperbenzoic acidHCID 962232-Oxocyclohexanepropiononitrile

생성물 2

HCID 4473-Chlorobenzoic AcidHCID 117689383-(7-Oxooxepan-2-yl)propanenitrile

시약·촉매·용매 1

HCID 8058Hexane용매2회

반응 조건

온도
55 °C

실험 절차

A reactor is loaded with 151 g of 3-(2-cyclohexanonyl)propionitrile in 500 ml of n-hexane and 260 g of m-chloroperbenzoic acid (70% titer) dissolved at 50° C. in 2000 ml of n-hexane in 30 minutes. The solution is heated to 55° C. for 15 hours. Cooling separates from the solution, in crystalline form, part of the m-chlorobenzoic acid, which is scarcely soluble in the system, together with a heavy liquid phase which is formed by 7-cyanoethyl-2-oxepanone and by m-chlorobenzoic acid. 71.5 g of 7-cyanoethyl-2-oxepanone, impure with m-chlorobenzoic acid, are recovered from the lower phase. 24 g of 7-cyanoethyl-2-oxepanone are recovered from the upper phase by concentration and by several crystallizations. Conversion with respect to the initial ketone is 85%. Yield on the converted substance is 57%.

후처리

  1. temperatureCooling

출처 및 근거

ORD 기록
ord-62b2e574547047a89abd0f996fcfb47e
출처 데이터셋
uspto-grants-1997_09
특허 번호
US05670661

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