Water → Methyl 2-amino-4,6-dimethoxybenzoate

HRID 749186ノート

反応式

HRID 749186 の反応式
S(OC)(O[CH3:5])(=O)=O.C(=O)([O-])[O-].[K+].[K+].[NH2:14][C:15]1[CH:23]=[C:22]([O:24][CH3:25])[CH:21]=[C:20]([O:26][CH3:27])[C:16]=1[C:17]([OH:19])=[O:18].O>CN(C)C=O>[NH2:14][C:15]1[CH:23]=[C:22]([O:24][CH3:25])[CH:21]=[C:20]([O:26][CH3:27])[C:16]=1[C:17]([O:19][CH3:5])=[O:18]

参加物

6

反応物 4

HCID 962WaterHCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 116584562-Amino-4,6-dimethoxybenzoic acid

生成物 1

HCID 11550253Methyl 2-amino-4,6-dimethoxybenzoate収率 77.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Dimethyl sulfate (1.04 ml, 11.0 mmol) was added dropwise to a mixture of potassium carbonate (3.34 g, 24.2 mmol) and 2-amino-4,6-dimethoxybenzoic acid (2.56 g, 11.0 mmol) in dimethylformamide (70 ml) at 0° C. The reaction was stirred for 1 hour, then poured into water. The resulting precipitate was filtered, washed with water and dried in vacuo. The filtrate was extracted with ethyl acetate, and the combined organic extracts were dried (magnesium sulphate) and concentrated in vacuo. The combined solids were dried in vacuo to yield methyl 2-amino-4,6-dimethoxybenzoate (1.8 g, 77% yield) as a yellow crystalline solid:

後処理

  1. filtrationThe resulting precipitate was filtered
  2. washwashed with water
  3. customdried in vacuo
  4. extractionThe filtrate was extracted with ethyl acetate
  5. dry with materialthe combined organic extracts were dried (magnesium sulphate)
  6. concentrationconcentrated in vacuo
  7. customThe combined solids were dried in vacuo

出典と根拠

ORDレコード
ord-14b32e1043484065b85d5420862f40b1
出典データセット
uspto-grants-2008_07
特許番号
US07402585B2

反応ノート

読み込み中…