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Water → HCID 76608131, 화합물

HRID 2099929
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HRID 2099929 반응식
[Cl:1][C:2]1[CH:23]=[C:22]([O:24][CH2:25][CH:26]=[C:27]([Cl:29])[Cl:28])[CH:21]=[C:20]([Cl:30])[C:3]=1[O:4][CH2:5][CH2:6][CH2:7][O:8][C:9]1[CH:14]=[CH:13][C:12]([C:15](=O)[CH2:16][O:17][CH3:18])=[CH:11][CH:10]=1.Cl.[CH3:32][O:33][NH2:34].C([O-])(=O)C.[Na+].O>CO>[CH3:32][O:33][N:34]=[C:15]([C:12]1[CH:13]=[CH:14][C:9]([O:8][CH2:7][CH2:6][CH2:5][O:4][C:3]2[C:2]([Cl:1])=[CH:23][C:22]([O:24][CH2:25][CH:26]=[C:27]([Cl:29])[Cl:28])=[CH:21][C:20]=2[Cl:30])=[CH:10][CH:11]=1)[CH2:16][O:17][CH3:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 517045Sodium AcetateHCID 521874O-Methylhydroxylamine hydrochlorideHCID 86602674HCID 86602674, 화합물

생성물 1

HCID 76608131HCID 76608131, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

296 mg of 1-(4-{3-[2,6-dichloro-4-(3,3-dichloro-allyloxy)-phenoxy]-propoxy}-phenyl)-2-methoxy-ethanone, 56 mg of O-methylhydroxylamine hydrochloride and 55 mg of sodium acetate are stirred in 4 ml of methanol at room temperature for 24 hours. The reaction mixture is poured into water and extracted with ethyl acetate. After concentration of the organic phases and purification over silica gel, the title compound is obtained in the form of an E/Z mixture. 1H-NMR (CDCl3) 300 MHz: 2.30 (m, 2H), 3.32+3.46 (s+s, 3H), 3.93+3.99 (s+s, 3H), 4.18 (t, 2H), 4.29 (m, 2H), 4.53-4.61 (m, 4H), 6.11 (t, 1H), 6.83 (s, 2H), 6.91 (d, 2H), 7.62 (d, 2H)

후처리

  1. extractionextracted with ethyl acetate
  2. customAfter concentration of the organic phases and purification over silica gel

출처 및 근거

ORD 기록
ord-885c4c28610949e79589db72dac97950
출처 데이터셋
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07569727B2

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