Iodine chloride → Methyl 4-amino-5-iodo-2-methoxybenzoate

HRID 630418노트

반응식

HRID 630418 반응식
[NH2:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[C:4]([O:12][CH3:13])[CH:3]=1.[I:14]Cl>C(O)(=O)C>[NH2:1][C:2]1[C:11]([I:14])=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[C:4]([O:12][CH3:13])[CH:3]=1

참가 물질

4

반응물 2

HCID 24640Iodine chlorideHCID 168705Methyl 4-amino-o-anisate

생성물 1

HCID 15700587Methyl 4-amino-5-iodo-2-methoxybenzoate수율 88%

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

실험 절차

To a solution of methyl 4-amino-2-methoxybenzoate (13 g, 0.07 mol) in acetic acid (300 mL) was added dropwise a solution of iodine monochloride (11.5 g, 0.07 mol) in acetic acid (50 mL). The mixture was stirred for 1.5 hours at room temperature. The precipitate was filtered and washed with ether. Then was dissolved with bicarbonate 4% and extracted with ethyl acetate. The organic layer was washed with brine, dried and the solvent was removed under reduced pressure giving the title compound as a white solid (88%), which was used in the next step without further purification.

후처리

  1. filtrationThe precipitate was filtered
  2. washwashed with ether
  3. dissolutionThen was dissolved with bicarbonate 4%
  4. extractionextracted with ethyl acetate
  5. washThe organic layer was washed with brine
  6. customdried
  7. customthe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-b0d898fe99ca41dcbd16a289f92af956
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09315463B2

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