Acetone → HCID 13657069, 화합물

HRID 745674

반응식

HRID 745674 반응식
[Cl:1][C:2]1[CH:19]=[C:18]([C:20]([F:23])([F:22])[F:21])[CH:17]=[CH:16][C:3]=1[O:4][C:5]1[CH:6]=[CH:7][C:8]([N+:13]([O-:15])=[O:14])=[C:9]([CH:12]=1)[CH2:10]Cl.[C:24]([O:34][CH2:35][CH3:36])(=[O:33])[CH:25]([CH2:27][C:28]([O:30][CH2:31][CH3:32])=[O:29])[OH:26].C(N(CC)CC)C.CC(C)=[O:46]>O>[CH2:35]([O:34][C:24]([CH:25]([O:26][C:10](=[O:46])[C:9]1[CH:12]=[C:5]([O:4][C:3]2[CH:16]=[CH:17][C:18]([C:20]([F:23])([F:22])[F:21])=[CH:19][C:2]=2[Cl:1])[CH:6]=[CH:7][C:8]=1[N+:13]([O-:15])=[O:14])[CH2:27][C:28]([O:30][CH2:31][CH3:32])=[O:29])=[O:33])[CH3:36]

참가 물질

6

반응물 4

HCID 180Acetone3회HCID 8471TriethylamineHCID 24197Diethyl malateHCID 13090781HCID 13090781, 화합물

생성물 1

HCID 13657069HCID 13657069, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a stirred solution of 5-[2-chloro-4-(trifluoromethyl)phenoxy]-2-nitrobenzyl chloride (3.8 g, 0.01 mole) in acetone (10 ml) was successively added diethyl DL malate (1.9 g, 0.01 mole) in acetone (10 ml) and triethylamine (1.01 g, 0.01 mole) in acetone (5 ml). A white precipitate quickly formed. The reaction was heated to reflux for 24 hours. Upon cooling, the reaction was poured in water (75 ml) and extracted twice with methylene chloride (25 ml@). The combined organic extracts were successively washed with 5% sodium hydroxide and brine solutions. The dried solution was stripped of solvent to give 3.5 g of an amber oil.

후처리

  1. customA white precipitate quickly formed
  2. temperatureThe reaction was heated
  3. temperatureto reflux for 24 hours
  4. temperatureUpon cooling
  5. extractionextracted twice with methylene chloride (25 ml@)
  6. washThe combined organic extracts were successively washed with 5% sodium hydroxide and brine solutions

출처 및 근거

ORD 기록
ord-b14a83937ea54b66b9bb63b80b93e972
출처 데이터셋
uspto-grants-1986_07
특허 번호
US04599442

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