2-Nitroanisole → Methyl alpha-chloro-3-methoxy-4-nitrophenylacetate

HRID 1018011

反応式

HRID 1018011 の反応式
CC(C)([O-])C.[K+].[N+:7]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[O:16][CH3:17])([O-:9])=[O:8].[Cl:18][CH:19](Cl)[C:20]([O:22][CH3:23])=[O:21]>C(O)(=O)C>[Cl:18][CH:19]([C:13]1[CH:14]=[CH:15][C:10]([N+:7]([O-:9])=[O:8])=[C:11]([O:16][CH3:17])[CH:12]=1)[C:20]([O:22][CH3:23])=[O:21]

参加物

5

反応物 3

HCID 70482-NitroanisoleHCID 8315Methyl dichloroacetateHCID 23665647Potassium tert-butoxide

生成物 1

HCID 10061131Methyl alpha-chloro-3-methoxy-4-nitrophenylacetate

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A suspension of potassium t-butoxide (1.44 kg) in dimethylformamide(6.61) cooled to −5° C. to −10° C., was treated with a mixture of 2-nitroanisole (690 g) and methyl dichloroacetate (915 g) over 4 hours, whilst maintaining the temperature below −5° C. The reaction mixture was then treated with acetic acid (770 ml) and then with water (6.61) and then e extracted three times with tert-butyl methyl ether (5.51). The combined extracts were washed with water (5.51), then with saturated sodium bicarbonate solution (5.51), then with saturated brine (5.51) and then dried over magnesium sulphate to give a solution of methyl α-chloro-3-methoxy-4-nitrophenylacetate.

後処理

  1. temperaturecooled to −5° C. to −10° C.
  2. temperaturewhilst maintaining the temperature below −5° C
  3. extractionwith water (6.61) and then e extracted three times with tert-butyl methyl ether (5.51)
  4. washThe combined extracts were washed with water (5.51)
  5. dry with materialwith saturated sodium bicarbonate solution (5.51), then with saturated brine (5.51) and then dried over magnesium sulphate

出典と根拠

ORDレコード
ord-4c4a2c05aa8c49e4a858341b89cd98bd
出典データセット
uspto-grants-2002_11
特許番号
US06479519B1

関連ノート

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