Methanol → HCID 67469370, 화합물

HRID 630419노트

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HRID 630419 반응식
[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

참가 물질

8

반응물 4

HCID 887MethanolHCID 962WaterHCID 15700587Methyl 4-amino-5-iodo-2-methoxybenzoate2회HCID 178514179HCID 178514179, 화합물

생성물 1

HCID 67469370HCID 67469370, 화합물수율 76%

시약·촉매·용매 3

HCID 178418397HCID 178418397, 화합물촉매HCID 3283Diethyl Ether용매HCID 6228Dimethylformamide용매

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온도
80 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-4c12ff883106411f8551a7e0b8f78730
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09315463B2

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