Sodium Carbonate → HCID 66748748、化合物

HRID 1748083ノート

反応式

HRID 1748083 の反応式
C(=O)([O-])[O-].[Na+].[Na+].[O:7]([C:14]1[CH:19]=[CH:18][C:17](B(O)O)=[CH:16][CH:15]=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.I[C:24]1[C:25]([NH2:32])=[N:26][CH:27]=[CH:28][C:29]=1[O:30][CH3:31]>COCCOC.O.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>[CH3:31][O:30][C:29]1[CH:28]=[CH:27][N:26]=[C:25]([NH2:32])[C:24]=1[C:17]1[CH:18]=[CH:19][C:14]([O:7][C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[CH:15][CH:16]=1

参加物

7

反応物 3

HCID 10340Sodium CarbonateHCID 27343774-Phenoxyphenylboronic acidHCID 242292063-Iodo-4-methoxypyridin-2-amine

生成物 1

HCID 66748748HCID 66748748、化合物収率 73.7%

試薬・触媒・溶媒 3

HCID 178418397HCID 178418397、化合物触媒HCID 962Water溶媒HCID 80711,2-Dimethoxyethane溶媒

反応条件

温度
80 °C

実験手順

A mixture of sodium carbonate (122 mg), tetrakis(triphenylphosphine)palladium(0) (33.2 mg), 4-phenoxyphenylboronic acid (160 mg) and 3-iodo-4-methoxypyridin-2-amine (144 mg) in DME (10 mL) and water (3 ml) was stirred at 80° C. overnight. The mixture was added with silica gel, concentrated in vacuo, and purified by column chromatography (silica gel, eluted with EtOAc in hexane) to give the title compound (124 mg) as a pale yellow solid.

後処理

  1. additionThe mixture was added with silica gel
  2. concentrationconcentrated in vacuo
  3. custompurified by column chromatography (silica gel, eluted with EtOAc in hexane)

出典と根拠

ORDレコード
ord-8b34129aeb634d14b661333773d40bd4
出典データセット
uspto-grants-2015_10
特許番号
US09150591B2

反応ノート

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