Chlorosuccinimide → 2-Chloro-N-hydroxy-benzamidine

HRID 2407656노트

반응식

HRID 2407656 반응식
[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]

참가 물질

5

반응물 2

HCID 31398ChlorosuccinimideHCID 96239o-Chlorobenzaldoxime

생성물 1

HCID 38097332-Chloro-N-hydroxy-benzamidine수율 99.6%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 15413tert-Butyl methyl ether용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3548018002b54ae2a6844f1eda82bdc4
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08809538B2

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