Tris(1,1-dimethylethyl)phosphine → 9-(4-[Benzoxazol-2-yl)phenyl]-3,6-diphenyl-9H-carbazole

HRID 1028870노트

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HRID 1028870 반응식
Br[C:2]1[CH:7]=[CH:6][C:5]([C:8]2[O:9][C:10]3[CH:16]=[CH:15][CH:14]=[CH:13][C:11]=3[N:12]=2)=[CH:4][CH:3]=1.[C:17]1([C:23]2[CH:24]=[CH:25][C:26]3[NH:27][C:28]4[C:33]([C:34]=3[CH:35]=2)=[CH:32][C:31]([C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)=[CH:30][CH:29]=4)[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.CC(C)([O-])C.[Na+].C(P(C(C)(C)C)C(C)(C)C)(C)(C)C>C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].C1(C)C=CC=CC=1.CCCCCC>[O:9]1[C:10]2[CH:16]=[CH:15][CH:14]=[CH:13][C:11]=2[N:12]=[C:8]1[C:5]1[CH:6]=[CH:7][C:2]([N:27]2[C:28]3[CH:29]=[CH:30][C:31]([C:36]4[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=4)=[CH:32][C:33]=3[C:34]3[C:26]2=[CH:25][CH:24]=[C:23]([C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=2)[CH:35]=3)=[CH:3][CH:4]=1

참가 물질

8

반응물 4

HCID 83681Tris(1,1-dimethylethyl)phosphineHCID 31232953,6-DiphenylcarbazoleHCID 128467152-(4-Bromophenyl)benzo(d)oxazoleHCID 23676156Sodium t-butoxide

생성물 1

HCID 582817999-(4-[Benzoxazol-2-yl)phenyl]-3,6-diphenyl-9H-carbazole

시약·촉매·용매 3

HCID 6505921(1E,4E)-1,5-diphenylpenta-1,4-dien-3-one; palladium촉매HCID 1140Toluene용매2회HCID 8058Hexane용매

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온도
80 °C

실험 절차

In a 100 mL three-neck flask were put 1.0 g (3.7 mmol) of 2-(4-bromophenyl)benzoxazole, 1.2 g (3.7 mmol) of 3,6-diphenyl-9H-carbazole, and 0.77 g (8.0 mmol) of sodium tert-butoxide. The atmosphere in the flask was replaced with nitrogen. To this mixture were added 15 mL of toluene and 0.10 mL of a 10% hexane solution of tri(tert-butyl)phosphine. This mixture was degassed by reducing the pressure in the flask by using an aspirator. After that, the atmosphere in the flask was replaced with nitrogen. To this mixture was added 0.030 g (0.052 mmol) of bis (dibenzylideneacetone)palladium(0), followed by stirring under a nitrogen stream at 80° C. for 5 hours. After that, toluene was added to this mixture, and this suspension was suction filtered through Celite 545 (produced by Kishida Chemical Co., Ltd., Catalog No. 020-14815), whereby a filtrate was obtained.

후처리

  1. customIn a 100 mL three-neck flask were put
  2. customThis mixture was degassed
  3. filtrationfiltered through Celite 545 (produced by Kishida Chemical Co., Ltd., Catalog No. 020-14815), whereby a filtrate
  4. customwas obtained

출처 및 근거

ORD 기록
ord-b67aa0056f514279bad981628d21f93c
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08735597B2

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