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Methyl iodide → Methyl 3-allyl-2-methoxy-4-amino-5-chlorobenzoate

HRID 2074006
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HRID 2074006 반응식
[C:1](=O)([O-])[O-].[K+].[K+].CI.[CH2:9]([C:12]1[C:13]([OH:24])=[C:14]([CH:19]=[C:20]([Cl:23])[C:21]=1[NH2:22])[C:15]([O:17][CH3:18])=[O:16])[CH:10]=[CH2:11]>CC(C)=O>[CH2:9]([C:12]1[C:13]([O:24][CH3:1])=[C:14]([CH:19]=[C:20]([Cl:23])[C:21]=1[NH2:22])[C:15]([O:17][CH3:18])=[O:16])[CH:10]=[CH2:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 14883228Methyl 3-allyl-2-hydroxy-4-amino-5-chlorobenzoate

생성물 1

HCID 14883229Methyl 3-allyl-2-methoxy-4-amino-5-chlorobenzoate

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of potassium carbonate (19 g), methyl iodide (8 g) and the phenolic compound of step 2 above (3.4 g) in acetone (100 ml) is stirred under reflux for about 6.4 hours. The mixture is partitioned between CH2Cl2 and H2O, and the organic layer is separated and washed with 10% aqueous HCl, dried (MgSO4) and evaporated affording an oil which chromatographed on silica gel affording the desired product which is used in the next step.

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후처리

  1. temperatureunder reflux for about 6.4 hours
  2. customThe mixture is partitioned between CH2Cl2 and H2O
  3. customthe organic layer is separated
  4. washwashed with 10% aqueous HCl
  5. dry with materialdried (MgSO4)
  6. customevaporated
  7. customaffording an oil which
  8. customchromatographed on silica gel affording the desired product which

출처 및 근거

ORD 기록
ord-b97d88257fa240919c5e7823ce7d5bc0
출처 데이터셋
uspto-grants-1990_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04920219

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