Methanol → Methyl 3-hydroxy-5-methoxy-4-nitrophenylacetate

HRID 1357863노트

반응식

HRID 1357863 반응식
[OH:1][C:2]1[CH:3]=[C:4]([CH2:13][C:14]([OH:16])=[O:15])[CH:5]=[C:6]([O:11][CH3:12])[C:7]=1[N+:8]([O-:10])=[O:9].[CH3:17]O>Cl>[OH:1][C:2]1[CH:3]=[C:4]([CH2:13][C:14]([O:16][CH3:17])=[O:15])[CH:5]=[C:6]([O:11][CH3:12])[C:7]=1[N+:8]([O-:10])=[O:9]

참가 물질

4

반응물 2

HCID 887MethanolHCID 181880853-Hydroxy-5-methoxy4-nitrophenylacetic acid

생성물 1

HCID 18188097Methyl 3-hydroxy-5-methoxy-4-nitrophenylacetate

시약·촉매·용매 1

HCID 313Hydrochloric Acid촉매

실험 절차

A solution of 3-hydroxy-5-methoxy-4-nitrophenylacetic acid (0.76 g, Reference Example 12) in methanol (100 mL) and concentrated hydrochloric acid (5 drops) was heated at reflux through 3A molecular sieve for 4 hours, then evaporated. The residue was partitioned between ethyl acetate and water. The organic phase was washed with water, then with brine, then dried and then evaporated. The residue was subjected to flash chromatography on silica eluting with dichloromethane, then with a mixture of methanol and dichloromethane (1:49, v/v) to give the title compound (0.34 g).

후처리

  1. customevaporated
  2. customThe residue was partitioned between ethyl acetate and water
  3. washThe organic phase was washed with water
  4. dry with materialwith brine, then dried
  5. customevaporated
  6. additionwith a mixture of methanol and dichloromethane (1:49, v/v)

출처 및 근거

ORD 기록
ord-6d09f92e665342db921d83f9643a269b
출처 데이터셋
uspto-grants-2003_07
특허 번호
US06593354B2

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