Potassium Phosphate, Tribasic → 4-Phenyldibenzofuran

HRID 717994

反応式

HRID 717994 の反応式
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

参加物

7

反応物 4

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

生成物 1

HCID 64257504-Phenyldibenzofuran

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 1140Toluene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-373797317bbe4301a53ec9f78b8163fc
出典データセット
uspto-grants-2015_11
特許番号
US09193745B2

関連ノート

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