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1,3-Bis(4-benzoylphenoxy)propane dioxime → 1,3-Bis[4-(alpha-aminobenzyl)phenoxy]propane

HRID 442246
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인쇄 미리보기

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HRID 442246 반응식
[C:1](=[N:34]O)([C:8]1[CH:33]=[CH:32][C:11]([O:12][CH2:13][CH2:14][CH2:15][O:16][C:17]2[CH:22]=[CH:21][C:20]([C:23](=[N:30]O)[C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)=[CH:19][CH:18]=2)=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H][H]>C(O)C.N.[Ni]>[NH2:30][CH:23]([C:20]1[CH:21]=[CH:22][C:17]([O:16][CH2:15][CH2:14][CH2:13][O:12][C:11]2[CH:10]=[CH:9][C:8]([CH:1]([NH2:34])[C:2]3[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=3)=[CH:33][CH:32]=2)=[CH:18][CH:19]=1)[C:24]1[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 867333991,3-Bis(4-benzoylphenoxy)propane dioximeHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 203406961,3-Bis[4-(alpha-aminobenzyl)phenoxy]propane

시약·촉매·용매 3

HCID 935Nickel촉매HCID 222Ammonia용매HCID 702Ethanol용매

실험 절차

The dioxime from Step 2 (20 g) is dissolved in ethyl alcohol saturated with ammonia gas (220 ml) and Raney nickel W-6 (2 g) added. The mixture is subjected to 500 psi hydrogen pressure and heated at 90° for four hours. The catalyst is removed by filtration and the solvent is removed by distillation to yield 15.5 g (83% of theory) of pale yellow crystals mp 118°-119°. Calculated for C29H30N2O2 : C, 79.42%; H, 6.90%; N, 6.39%. Found: C, 79.14% H, 6.57%; N, 6.89%.

후처리

  1. addition(2 g) added
  2. temperatureheated at 90° for four hours
  3. customThe catalyst is removed by filtration
  4. customthe solvent is removed by distillation

출처 및 근거

ORD 기록
ord-b0cf2c87c5de4c02a8ca3b54edca7351
출처 데이터셋
uspto-grants-1977_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04044139

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