Methanol → HCID 67469370、化合物

HRID 630419ノート

反応式

HRID 630419 の反応式
[NH2:1][C:2]1[C:11](I)=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[C:4]([O:13][CH3:14])[CH:3]=1.[C:15]([Zn]C#N)#[N:16].O.CO>CN(C)C=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.CCOCC>[NH2:1][C:2]1[C:11]([C:15]#[N:16])=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[C:4]([O:13][CH3:14])[CH:3]=1

参加物

8

反応物 4

HCID 887MethanolHCID 962WaterHCID 15700587Methyl 4-amino-5-iodo-2-methoxybenzoate2 回HCID 178514179HCID 178514179、化合物

生成物 1

HCID 67469370HCID 67469370、化合物収率 76%

試薬・触媒・溶媒 3

HCID 178418397HCID 178418397、化合物触媒HCID 3283Diethyl Ether溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

A solution of methyl 4-amino-5-iodo-2-methoxybenzoate (intermediate 128; 5 g, 16.28 mmol) and dicyanozinc (1.5 g, 12.77 mmol) in dimethylformamide (50 mL) in a slenck vessel was degasified with nitrogen. Then tetrakis (1 g, 0.87 mmol) was added and the reaction mixture was stirred at 80° C. for 2 hours. Water was added into the reaction mixture and the crude was extracted with ethyl acetate, the organic layer was washed with brine, dried and the solvent was removed under reduced pressure. The crude obtained was treated with methanol and ether to obtain the title compound as a yellow solid (76%).

後処理

  1. extractionthe crude was extracted with ethyl acetate
  2. washthe organic layer was washed with brine
  3. customdried
  4. customthe solvent was removed under reduced pressure
  5. customThe crude obtained

出典と根拠

ORDレコード
ord-4c12ff883106411f8551a7e0b8f78730
出典データセット
uspto-grants-2016_04
特許番号
US09315463B2

反応ノート

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