Hydrochloric Acid → 2-Chloroacetylamino-5-ethoxycarbonyl-4,6-dimethylbenzoic acid

HRID 1680836ノート

反応式

HRID 1680836 の反応式
[NH2:1][C:2]1[CH:10]=[C:9]([CH3:11])[C:8]([C:12]([O:14][CH2:15][CH3:16])=[O:13])=[C:7]([CH3:17])[C:3]=1[C:4]([OH:6])=[O:5].N1C=CC=CC=1.[Cl:24][CH2:25][C:26](Cl)=[O:27].Cl>C1C=CC=CC=1>[Cl:24][CH2:25][C:26]([NH:1][C:2]1[CH:10]=[C:9]([CH3:11])[C:8]([C:12]([O:14][CH2:15][CH3:16])=[O:13])=[C:7]([CH3:17])[C:3]=1[C:4]([OH:6])=[O:5])=[O:27]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 6577Chloroacetyl chlorideHCID 126858402-Amino-5-ethoxycarbonyl-4,6-dimethylbenzoic acid

生成物 1

HCID 129124362-Chloroacetylamino-5-ethoxycarbonyl-4,6-dimethylbenzoic acid

試薬・触媒・溶媒 1

HCID 241Benzene溶媒2 回

実験手順

To an ice-cooled mixture consisting of 0.8 g of 2-amino-5-ethoxycarbonyl-4,6-dimethylbenzoic acid, 20 ml of dry benzene, and 0.5 ml of pyridine was added dropwise with stirring a solution of 0.4 ml of chloroacetyl chloride in 5 ml of benzene. The mixture was stirred overnight and then, shaken with dilute hydrochloric acid. The layers were separated. The aqueous layer was extracted with ethyl acetate, and the combined organic extracts were washed with water, dried over sodium sulfate, and evaporated. The residue was recrystallized from ethyl ether/n-hexane to give 0.65 g of 2-chloroacetylamino-5-ethoxycarbonyl-4,6-dimethylbenzoic acid (m.p. 124°-125° C.).

後処理

  1. additionwas added dropwise
  2. customThe layers were separated
  3. extractionThe aqueous layer was extracted with ethyl acetate
  4. washthe combined organic extracts were washed with water
  5. dry with materialdried over sodium sulfate
  6. customevaporated
  7. customThe residue was recrystallized from ethyl ether/n-hexane

出典と根拠

ORDレコード
ord-ed721349c55e4a99ada2ecf3e4faa220
出典データセット
uspto-grants-1981_06
特許番号
US04276295

反応ノート

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