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Hexane → HCID 57617105, 화합물

HRID 389187
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HRID 389187 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]
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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

반응 조건

온도
300 °C

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 portionwise, and the mixture stirred at reflux for 30 minutes after addition was complete. The mixture was cooled to RT; hexane (400 mL) was added; and the mixture was stirred for 30 minutes, filtered, and the solids washed with hexane to give the title compound (38 g). LRMS (M+H)+ Calcd.: 330.0; found 330.2.

후처리

  1. temperatureat reflux for 30 minutes
  2. additionafter addition
  3. temperatureThe mixture was cooled to RT
  4. stirringand the mixture was stirred for 30 minutes
  5. filtrationfiltered
  6. washthe solids washed with hexane

출처 및 근거

ORD 기록
ord-2b3a735fff97402f98584df7c705a2c4
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08377874B2

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