Sodium Carbonate → 4-Phenylquinazoline-6-carbaldehyde

HRID 2261086

反応式

HRID 2261086 の反応式
Cl[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([CH:12]=[O:13])[CH:10]=2)[N:5]=[CH:4][N:3]=1.[C:14]1(B(O)O)[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.C(=O)([O-])[O-].[Na+].[Na+]>C1(C)C=CC=CC=1.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[C:14]1([C:2]2[C:11]3[C:6](=[CH:7][CH:8]=[C:9]([CH:12]=[O:13])[CH:10]=3)[N:5]=[CH:4][N:3]=2)[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

参加物

6

反応物 3

HCID 10340Sodium CarbonateHCID 66827Phenylboronic AcidHCID 574696394-Chloroquinazoline-6-carbaldehyde

生成物 1

HCID 574696424-Phenylquinazoline-6-carbaldehyde

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒HCID 1140Toluene溶媒

実験手順

4-Chloro-quinazoline-6-carbaldehyde (50 mg, 0.26 mmol), Pd(PPh3)4 (13 mg, 0.01 mmol), phenylboronic acid (63 mg, 0.52 mmol) and sodium carbonate (sat. sol: 50 ul) were heated up in toluene at 100° C. for 12 h. After evaporation of the solvents, the residue was taken up in ethyl acetate and washed with brine twice. Organic phases were then concentrated and raw materiel was purified on silica gel using DCM/EtOH 95:5 as eluents to give 50 mgs (82%) of the desired cpd with a 85% purity.

後処理

  1. customAfter evaporation of the solvents
  2. washwashed with brine twice
  3. concentrationOrganic phases were then concentrated
  4. customraw materiel was purified on silica gel
  5. customto give 50 mgs (82%) of the desired cpd with a 85% purity

出典と根拠

ORDレコード
ord-5e88d90cef514a25b7957a759eba3ce5
出典データセット
uspto-grants-2010_12
特許番号
US07846925B2

関連ノート

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