Chlorosuccinimide → 2-Chloro-N-hydroxy-benzamidine

HRID 2407656ノート

反応式

HRID 2407656 の反応式
[Cl:1]N1C(=O)CCC1=O.[Cl:9][C:10]1[CH:18]=[CH:17][CH:16]=[CH:15][C:11]=1[CH:12]=[N:13][OH:14]>CN(C)C=O.C(OC)(C)(C)C>[Cl:9][C:10]1[CH:18]=[CH:17][CH:16]=[CH:15][C:11]=1[C:12]([Cl:1])=[N:13][OH:14]

参加物

5

反応物 2

HCID 31398ChlorosuccinimideHCID 96239o-Chlorobenzaldoxime

生成物 1

HCID 38097332-Chloro-N-hydroxy-benzamidine収率 99.6%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 15413tert-Butyl methyl ether溶媒

実験手順

N-Chlorosuccinimide (56.1 g) was added slowly to a 0° C. solution of the compound prepared in Example 4 (65.4 g) in N,N-dimethylformamide (1.2 L). The reaction was stirred at room temperature overnight and then diluted with ice water and methyl tert-butyl ether. The layers were separated and the aqueous phase was extracted once more with methyl tert-butyl ether. The organic phases were combined, washed with brine, dried over anhydrous magnesium sulfate and concentrated to obtain the title compound (79.5 g) having the following physical data.

後処理

  1. customThe layers were separated
  2. extractionthe aqueous phase was extracted once more with methyl tert-butyl ether
  3. washwashed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-3548018002b54ae2a6844f1eda82bdc4
出典データセット
uspto-grants-2014_08
特許番号
US08809538B2

反応ノート

読み込み中…