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Hexane → HCID 57617105, 화합물

HRID 2045697
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HRID 2045697 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)=[CH:10][C:11]([O:13]CC)=O)=[CH:4][C:3]=1[O:22][CH3:23].CCCCCC>C1C=CC(C2C=CC=CC=2)=CC=1.C1C=CC(OC2C=CC=CC=2)=CC=1>[Br:1][C:2]1[CH:7]=[C:6]2[C:5](=[CH:4][C:3]=1[O:22][CH3:23])[NH:8][C:9]([C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1)=[CH:10][C:11]2=[O:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 8058HexaneHCID 58005168Ethyl 3-[(4-bromo-3-methoxyphenyl)amino]-3-phenylacrylate

생성물 1

HCID 57617105HCID 57617105, 화합물수율 88.5%

시약·촉매·용매 1

HCID 246701,1'-Biphenyl, mixt. with 1,1'-oxybis(benzene)용매3회

실험 절차

DOWTHERM A (450 mL) was heated to reflux (˜300 C). A mixture of the product from step 2 (49 g, 130 mmol) in DOWTHERM A (50 mL) was added to the heated DOWTHERM A solution portionwise. The mixture was stirred at reflux for 30 min after the addition was complete. The mixture was cooled RT, and hexane (400 mL) was added. The mixture was stirred for 30 min and filtered, and the solids were washed with hexane to give the title compound (38 g, 88% yield). LRMS (M+H)+ Calcd.: 330.0; found 330.2.

후처리

  1. temperatureto reflux (˜300 C)
  2. temperatureat reflux for 30 min
  3. additionafter the addition
  4. stirringThe mixture was stirred for 30 min
  5. filtrationfiltered
  6. washthe solids were washed with hexane

출처 및 근거

ORD 기록
ord-d0bbaba9470b47b2b146dfb92ba4ccee
출처 데이터셋
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08591878B2

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