3-Benzyloxypyridine → N-amino-3-benzyloxypyridinium mesitylenesulfonate

HRID 1590113ノート

反応式

HRID 1590113 の反応式
[C:1]1([CH3:14])[CH:6]=[C:5]([CH3:7])[CH:4]=[C:3]([CH3:8])[C:2]=1[S:9]([O:12][NH2:13])(=[O:11])=[O:10].[CH2:15]([O:22][C:23]1[CH:24]=[N:25][CH:26]=[CH:27][CH:28]=1)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1>C(Cl)Cl>[C:1]1([CH3:14])[CH:6]=[C:5]([CH3:7])[CH:4]=[C:3]([CH3:8])[C:2]=1[S:9]([O-:12])(=[O:11])=[O:10].[NH2:13][N+:25]1[CH:26]=[CH:27][CH:28]=[C:23]([O:22][CH2:15][C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=2)[CH:24]=1

参加物

4

反応物 2

HCID 100126353-BenzyloxypyridineHCID 11830845O-(2,4,6-Trimethylbenzenesulfonyl)hydroxylamine

生成物 1

HCID 15257892N-amino-3-benzyloxypyridinium mesitylenesulfonate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of O-mesitylenesulfonylhydroxylamine (13.7 g, 44.6 mmole, purity of 70%) in methylene chloride (150 ml) was added dropwise to a solution of 3-benzyloxypyridine (8.25 g, 44.6 mmole) in methylene chloride (150 ml) under ice-cooling, with stirring. The reaction solution was returned to room temperature, stirred for 1 hours and concentrated to one-quarter of the original volume at 20° to 30° C., and ether was added to the concentrate, thereby white crystals were precipitated. This product was used in the next reaction, without being purified.

後処理

  1. temperaturecooling
  2. customwas returned to room temperature
  3. stirringstirred for 1 hours
  4. concentrationconcentrated to one-quarter of the original volume at 20° to 30° C.
  5. additionether was added to the concentrate
  6. customwhite crystals were precipitated
  7. customThis product was used in the next reaction
  8. customwithout being purified

出典と根拠

ORDレコード
ord-a37ccfad46eb4f3ca7b8a6def85f67d4
出典データセット
uspto-grants-1993_04
特許番号
US05202334

反応ノート

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