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(4-Aminophenoxy)benzene → HCID 21082455, 화합물

HRID 347290
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HRID 347290 반응식
C(O[C:4](=[O:27])[C:5]([NH:7][C:8]1[CH:13]=[CH:12][C:11]([O:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26])=[CH:10][CH:9]=1)=[O:6])C.[O:28]([C:35]1[CH:41]=[CH:40][C:38]([NH2:39])=[CH:37][CH:36]=1)[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1.CC(C)([O-])C.[Li+]>C1(C)C(C)=CC=CC=1>[CH2:15]([O:14][C:11]1[CH:10]=[CH:9][C:8]([NH:7][C:5](=[O:6])[C:4]([NH:39][C:38]2[CH:37]=[CH:36][C:35]([O:28][C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=3)=[CH:41][CH:40]=2)=[O:27])=[CH:13][CH:12]=1)[CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8764(4-Aminophenoxy)benzeneHCID 236647642-Propanol, 2-methyl-, lithium salt (1:1)HCID 58800192HCID 58800192, 화합물

생성물 1

HCID 21082455HCID 21082455, 화합물수율 85.6%

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

A solution of N-(4-dodecyloxyphenyl)oxalamic acid ethyl ester (10 g, 0.026 mol), 4-phenoxyaniline (5 g, 0.026 mol) and lithium t-butoxide (0.2 g, 0.0026 mol) in xylene (50 mL) isheated to gentle reflux. A distillate of ethanol/xylene is slowly collected; the reaction volumn is kept at 50 mL by adding xylene. Heating and distillation continued for 3 hours. The reaction mixture is cooled, the solids are collected and washed sequentially with warm ethyl acetate, ethanol, water and finally ethanol. There is obtained 11.5 g white solid mp: 179–181.

후처리

  1. distillationA distillate of ethanol/xylene is slowly collected
  2. additionby adding xylene
  3. temperatureHeating
  4. distillationdistillation
  5. temperatureThe reaction mixture is cooled
  6. customthe solids are collected
  7. washwashed sequentially with warm ethyl acetate, ethanol, water and finally ethanol

출처 및 근거

ORD 기록
ord-c83d14d0d1a1466eb5aa57dc263e76ab
출처 데이터셋
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07173128B2

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