Lamotrigine → Lamotrigine N-Acetate

HRID 745913

反応式

HRID 745913 の反応式
[NH2:1][C:2]1[N:3]=[N:4][C:5]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([Cl:15])[C:10]=2[Cl:16])=[C:6]([NH2:8])[N:7]=1.[C:17](OC(=O)C)(=[O:19])[CH3:18]>C(O)(=O)C>[C:17]([NH:8][C:6]1[N:7]=[C:2]([NH2:1])[N:3]=[N:4][C:5]=1[C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([Cl:15])[C:10]=1[Cl:16])(=[O:19])[CH3:18]

参加物

4

反応物 2

HCID 3878LamotrigineHCID 7918Acetic Anhydride

生成物 1

HCID 23311124Lamotrigine N-Acetate

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A solution of 3,5-diamino-6-(2,3-dichlorophenyl)-1,2,4-triazine (2 gm, 8 mM) and acetic anhydride (10 mls) in acetic acid (20 mls) was stirred and heated to reflux for 2 hours. The solution was then cooled and evaporated down in vacuo. The residue was treated with aqueous 0.880 ammonia (100 mls) and the resultant mixture was stirred for 2 hours. The solid was separated by filtration, dried then recrystallized from isopropanol to give 5-acetamido-3-amino-6-(2,3-dichlorophenyl)-1,2,4-triazine. Yield 1.0 gms (42%), m.p. 250°-252° (uncorrected).

後処理

  1. temperatureheated
  2. temperatureto reflux for 2 hours
  3. temperatureThe solution was then cooled
  4. customevaporated down in vacuo
  5. additionThe residue was treated with aqueous 0.880 ammonia (100 mls)
  6. customThe solid was separated by filtration
  7. customdried
  8. customthen recrystallized from isopropanol

出典と根拠

ORDレコード
ord-7946c915cc52429ea103b3d1e9015bf0
出典データセット
uspto-grants-1986_07
特許番号
US04602017

関連ノート

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