Potassium Phosphate, Tribasic → 4-Phenyldibenzofuran

HRID 717994

반응식

HRID 717994 반응식
I[C:2]1[C:7]2[O:8][C:9]3[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=3[C:6]=2[CH:5]=[CH:4][CH:3]=1.[C:15]1(B(O)O)[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.C1(P(C2CCCCC2)C2C=CC=CC=2C2C(OC)=CC=CC=2OC)CCCCC1.[O-]P([O-])([O-])=O.[K+].[K+].[K+]>O.C1(C)C=CC=CC=1>[C:15]1([C:2]2[C:7]3[O:8][C:9]4[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=4[C:6]=3[CH:5]=[CH:4][CH:3]=2)[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1

참가 물질

7

반응물 4

HCID 62657Potassium Phosphate, TribasicHCID 66827Phenylboronic AcidHCID 4582574-IododibenzofuranHCID 112698722-Dicyclohexylphosphino-2',6'-dimethoxybiphenyl

생성물 1

HCID 64257504-Phenyldibenzofuran

시약·촉매·용매 2

HCID 962Water용매HCID 1140Toluene용매

실험 절차

4-iododibenzo[b,d]furan (4 g, 13.60 mmol), phenylboronic acid (1.99 g, 16.32 mmol), dicyclohexyl(2′,6′-dimethoxy-[1,1′-biphenyl]-2-yl)phosphine (0.447 g, 1.08 mmol), Pd2(dba)2 (0.250 g, 0.272 mmol), K3PO4 (10.1 g, 47.6 mmol), 150 mL toluene and 15 mL water were charged in a 250 mL flask. The reaction mixture was degassed by bubbling N2 for 30 minutes and then heated to reflux under N2 overnight. The reaction was cooled to room temperature and the crude product was purified by silica gel column to yield 3.3 g (99%), which was confirmed by GC-MS.

후처리

  1. customThe reaction mixture was degassed
  2. customby bubbling N2 for 30 minutes
  3. temperatureheated
  4. temperatureto reflux under N2 overnight
  5. customthe crude product was purified by silica gel column
  6. customto yield 3.3 g (99%), which

출처 및 근거

ORD 기록
ord-373797317bbe4301a53ec9f78b8163fc
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09193745B2

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