Sodium Carbonate → HCID 23687032、化合物

HRID 727440ノート

反応式

HRID 727440 の反応式
[NH2:1][C:2]1[C:7](I)=[CH:6][C:5]([Br:9])=[CH:4][C:3]=1[S:10]([OH:13])(=[O:12])=[O:11].[S:14]1[CH:18]=[CH:17][CH:16]=[C:15]1B(O)O.C(=O)([O-])[O-].[Na+:26].[Na+]>COCCOC.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>[NH2:1][C:2]1[C:7]([C:15]2[S:14][CH:18]=[CH:17][CH:16]=2)=[CH:6][C:5]([Br:9])=[CH:4][C:3]=1[S:10]([O-:13])(=[O:12])=[O:11].[Na+:26]

参加物

6

反応物 3

HCID 10340Sodium CarbonateHCID 27339602-Thiopheneboronic acidHCID 189193852-Amino-5-bromo-3-iodobenzenesulphonic acid

生成物 1

HCID 23687032HCID 23687032、化合物

試薬・触媒・溶媒 2

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

反応条件

温度
0 °C

実験手順

A mixture of 36 g (95.3 mmol) of 2-amino-5-bromo-3-iodobenzenesulphonic acid and 12.2 g (95.3 mmol) of 2-thienylboronic acid in 140 ml of 1,2-dimethoxyethane in the presence of 5.5 g of tetrakis(triphenylphosphine)palladium (0) and 30.3 g of sodium carbonate is heated at 70°-75° C. for 8.5 hours. The solvent is evaporated off under vacuum, the mixture is cooled to 0° C. and washed with water to pH=7, and the residue is then taken up in an ether/ethanol mixture (95:5).

後処理

  1. temperatureis heated at 70°-75° C. for 8.5 hours
  2. customThe solvent is evaporated off under vacuum
  3. washwashed with water to pH=7

出典と根拠

ORDレコード
ord-2536f492f1304a019258011950e887e6
出典データセット
uspto-grants-1998_01
特許番号
US05712393

反応ノート

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