Hydroxyamine hydrochloride → 4-(2,4-Difluorobenzoyl)-1-formylpiperidine oxime

HRID 370885노트

반응식

HRID 370885 반응식
C([O-])(=O)C.[NH4+:5].[F:6][C:7]1[CH:22]=[C:21]([F:23])[CH:20]=[CH:19][C:8]=1[C:9]([CH:11]1[CH2:16][CH2:15][N:14]([CH:17]=O)[CH2:13][CH2:12]1)=[O:10].Cl.N[OH:26]>O.C(O)C>[F:6][C:7]1[CH:22]=[C:21]([F:23])[CH:20]=[CH:19][C:8]=1[C:9]([CH:11]1[CH2:16][CH2:15][N:14]([CH:17]=[N:5][OH:26])[CH2:13][CH2:12]1)=[O:10]

참가 물질

6

반응물 3

HCID 443297Hydroxyamine hydrochlorideHCID 517165Ammonium AcetateHCID 114141024-(2,4-Difluorobenzoyl)piperidine-1-carbaldehyde

생성물 1

HCID 867386014-(2,4-Difluorobenzoyl)-1-formylpiperidine oxime수율 75.5%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

A solution of 12 g of ammonium acetate in 45 ml of water was added to a solution of 15 g of 4-(2,4-difluorobenzoyl)-1-formylpiperidine and 6 g of hydroxylamine hydrochloride in 35 ml of ethanol. The mixture was heated for 18 hrs at 90°, with stirring. The solvent was evaporated in vacuum until precipitation occurred. Water (500 ml) was added. The mixture was filtered, washed with 300 ml of water and dried in vacuum over phosphorous pentoxide to yield 12 g (75.5%) of product. Recrystallization from ethanol and water yielded the analytical sample, mp, 185°.

후처리

  1. temperatureThe mixture was heated for 18 hrs at 90°
  2. customThe solvent was evaporated in vacuum until precipitation
  3. additionWater (500 ml) was added
  4. filtrationThe mixture was filtered
  5. washwashed with 300 ml of water
  6. dry with materialdried in vacuum over phosphorous pentoxide

출처 및 근거

ORD 기록
ord-4bf1fa9fe09a44149b7ab77ef4aad8b1
출처 데이터셋
uspto-grants-1985_07
특허 번호
US04528376

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