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Triethyl Phosphate → Dibenzo(a,C)carbazole

HRID 1914408
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HRID 1914408 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[C:10]1[C:11]2[C:16]([C:17]3[CH:18]=[CH:19][CH:20]=[CH:21][C:22]=3[CH:23]=1)=[CH:15][CH:14]=[CH:13][CH:12]=2)([O-])=O.P(OCC)(OCC)(OCC)=O>O>[CH:21]1[C:22]2[C:23]3[NH:1][C:4]4[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=4[C:10]=3[C:11]3[C:16](=[CH:15][CH:14]=[CH:13][CH:12]=3)[C:17]=2[CH:18]=[CH:19][CH:20]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6535Triethyl PhosphateHCID 58410431HCID 58410431, 화합물

생성물 1

HCID 155584Dibenzo(a,C)carbazole수율 47%

시약·촉매·용매 1

HCID 962Water용매

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온도
150 °C

실험 절차

Next, a mixed solution of 2.0 g of 9-(2-nitrophenyl)phenanthrene and 40 ml of triethyl phosphate was heated and stirred under a nitrogen gas stream at 150° C. for 8 hours. After cooling to room temperature, 50 ml of water was poured into the solution, followed by extraction with 50 ml of toluene. The organic layer was washed twice with 50 ml of water, dried over magnesium sulfate and then concentrated by evaporation. The concentrate was purified by silica gel chromatography and then vacuum-dried to obtain 840 mg of 13H-13-azaindeno[1,2-l]phenanthrene.

후처리

  1. temperatureAfter cooling to room temperature
  2. extractionfollowed by extraction with 50 ml of toluene
  3. washThe organic layer was washed twice with 50 ml of water
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated by evaporation
  6. customThe concentrate was purified by silica gel chromatography
  7. customvacuum-dried

출처 및 근거

ORD 기록
ord-8ff2a2ba7d5c4f809a65fa3a6850152e
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08610345B2

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