Hydroxylamine → 2,3-Difluoro-6-(trifluoromethyl)benzamide

HRID 322217

반응식

HRID 322217 반응식
C[OH:2].[OH2:3].[NH2:4]O.[F:6][C:7]1[C:14]([F:15])=[CH:13][CH:12]=[C:11]([C:16]([F:19])([F:18])[F:17])[C:8]=1[C:9]#[N:10]>O>[F:6][C:7]1[C:14]([F:15])=[CH:13][CH:12]=[C:11]([C:16]([F:19])([F:17])[F:18])[C:8]=1[C:9](=[N:4][OH:3])[NH2:10].[F:6][C:7]1[C:14]([F:15])=[CH:13][CH:12]=[C:11]([C:16]([F:19])([F:17])[F:18])[C:8]=1[C:9]([NH2:10])=[O:2]

참가 물질

6

반응물 3

HCID 787HydroxylamineHCID 101044562,3-Difluoro-6-(trifluoromethyl)benzonitrileHCID 22242641Methanol--water (1/1)

생성물 2

HCID 220101192,3-Difluoro-6-(trifluoromethyl)benzamideHCID 544182132,3-Difluoro-N-hydroxy-6-(trifluoromethyl)benzimidamide

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

Into an SUS reaction vessel was placed a mixed solvent of 1.5 L of methanol-water (volume ratio 1:2, the same tap water as that used in Example 2 was used as water) into which 99.09 g (1.50 mol) of 50% hydroxylamine aqueous solution was dissolved beforehand. Into the mixed solvent was added 103.56 g (500 mmol) of 2,3-difluoro-6-trifluoromethylbenzonitrile (I″). The reaction temperature stood at 60° C. for 7 hours and was returned to room temperature. In HPLC analysis of the reaction solution, it was shown that (I″) disappeared, 2,3-difluoro-6-trifluoromethylbenzamidoxime (II′) was mainly produced (yield 63.2%) and 2,3-difluoro-6-trifluoromethylbenzamide (III′) was noticeably produced as a byproduct (yield 16.6%).

후처리

  1. customInto an SUS reaction vessel was placed
  2. dissolutionwas dissolved beforehand
  3. customwas returned to room temperature

출처 및 근거

ORD 기록
ord-84d0e60dca374dd68ebd4b766ca4f0a7
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06211232B1

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