Hydroxyamine hydrochloride → HCID 86752926, 화합물

HRID 1957259노트

반응식

HRID 1957259 반응식
[Cl:1][C:2]1[C:3]([C:12]2[CH:17]=[CH:16][C:15]([Cl:18])=[C:14]([CH:19]=O)[CH:13]=2)=[N:4][CH:5]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:7]=1.C(=O)(O)[O-].[Na+].Cl.[NH2:27][OH:28]>O1CCCC1>[Cl:1][C:2]1[C:3]([C:12]2[CH:17]=[CH:16][C:15]([Cl:18])=[C:14]([CH:19]=[N:27][OH:28])[CH:13]=2)=[N:4][CH:5]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:7]=1

참가 물질

5

반응물 3

HCID 443297Hydroxyamine hydrochlorideHCID 516892Sodium BicarbonateHCID 186929322-Chloro-5-[3-chloro-5-(trifluoromethyl)pyridin-2-yl]benzaldehyde

생성물 1

HCID 86752926HCID 86752926, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

22.6 g of 3-chloro-2-(4-chloro-3-formylphenyl)-5-trifluoromethylpyridine, 6.5 g of sodium bicarbonate and 5.4 g of hydroxylamine hydrochloride in 100 ml of tetrahydrofuran were stirred at 23° C. for 24 hours. The tetrahydrofuran was then removed, after which the residue was taken up in 100 ml of methylene chloride. The solution was washed twice with 100 ml of water. The solid formed during this was removed, washed with water and dried. Concentration of the organic phase resulted in a residue which was purified by chromatography on silica gel with cyclohexane/ethyl acetate (7:3). Yield: 26.1 g (82%) of colorless crystals; melting point: 173°-174° C.

후처리

  1. customThe tetrahydrofuran was then removed
  2. washThe solution was washed twice with 100 ml of water
  3. customThe solid formed during
  4. customthis was removed
  5. washwashed with water
  6. customdried
  7. customConcentration of the organic phase resulted in a residue which
  8. customwas purified by chromatography on silica gel with cyclohexane/ethyl acetate (7:3)

출처 및 근거

ORD 기록
ord-5ab8592f646b46b2be451895b282f07a
출처 데이터셋
uspto-grants-1998_07
특허 번호
US05783522

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