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

HRID 1357863ノート

反応式

HRID 1357863 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid触媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-6d09f92e665342db921d83f9643a269b
出典データセット
uspto-grants-2003_07
特許番号
US06593354B2

反応ノート

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