HCID 58629740、化合物 → HCID 58629777、化合物

HRID 423261ノート

反応式

HRID 423261 の反応式
[CH3:1][O:2][C:3](=[O:17])[C:4]1[CH:9]=[C:8]([O:10][CH3:11])[C:7]([O:12][CH2:13][O:14][CH3:15])=[C:6](I)[CH:5]=1.[CH3:18][Zn]C.C1COCC1>C1COCC1.C(OCC)(=O)C.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>[CH3:1][O:2][C:3](=[O:17])[C:4]1[CH:5]=[C:6]([CH3:18])[C:7]([O:12][CH2:13][O:14][CH3:15])=[C:8]([O:10][CH3:11])[CH:9]=1

参加物

6

反応物 2

HCID 58629740HCID 58629740、化合物HCID 178420677HCID 178420677、化合物

生成物 1

HCID 58629777HCID 58629777、化合物

試薬・触媒・溶媒 3

HCID 178418397HCID 178418397、化合物触媒HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
80 °C

実験手順

To a solution of 3-iodo-5-methoxy-4-methoxymethoxybenzoic acid methyl ester (700 mg) in THF (7 mL) were added tetrakis(triphenylphosphine)palladium(0) (115 mg) and 2M dimethylzinc/THF solution (1.20 mL), and the mixture was stirred at 80° C. for 30 minutes. The reaction solution was diluted with ethyl acetate, washed with 1N hydrochloric acid, water, and saturated brine, dried over anhydrous sodium sulfate, and concentrated in vacuo to give the title compound (767 mg) as a crude purified product of pale yellow oil.

後処理

  1. washwashed with 1N hydrochloric acid, water, and saturated brine
  2. dry with materialdried over anhydrous sodium sulfate
  3. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-7b12c58f793d4e59befb3ec9ed4bc0ea
出典データセット
uspto-grants-2012_01
特許番号
US08101774B2

反応ノート

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