Hydroxyamine hydrochloride → HCID 86752926、化合物

HRID 1957259ノート

反応式

HRID 1957259 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 86752926HCID 86752926、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-5ab8592f646b46b2be451895b282f07a
出典データセット
uspto-grants-1998_07
特許番号
US05783522

反応ノート

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