Phosphorus oxychloride → 2-Hydroxy-3,5-diisopropyl benzonitrile

HRID 1272265노트

반응식

HRID 1272265 반응식
P(Cl)(Cl)(Cl)=O.[CH:6]([C:9]1[CH:17]=[C:16]([CH:18]([CH3:20])[CH3:19])[CH:15]=[C:11]([C:12]([NH2:14])=O)[C:10]=1[OH:21])([CH3:8])[CH3:7]>N1C=CC=CC=1>[OH:21][C:10]1[C:9]([CH:6]([CH3:7])[CH3:8])=[CH:17][C:16]([CH:18]([CH3:20])[CH3:19])=[CH:15][C:11]=1[C:12]#[N:14]

참가 물질

4

반응물 2

HCID 24813Phosphorus oxychlorideHCID 184569023,5-Diisopropyl salicylamide

생성물 1

HCID 184569012-Hydroxy-3,5-diisopropyl benzonitrile수율 60%

시약·촉매·용매 1

HCID 1049Pyridine용매2회

실험 절차

To a solution of phosphorous oxychloride (1.35 g, 8.8 mmole) and dry pyridine (12 mL) cooled to 0° C., a solution of 3,5-diisopropyl salicylamide (1.10 g, 5 mmole) and dry pyridine (5 mL) was slowly added drop by drop. The reaction mixture was stirred at room temperature, whereat the colour changed from colourless over violet to red. After extraction with ethyl acetate and washing with a saturated sodium chloride solution and 2N hydrochloric acid, the organic layer was dried and evaporated under reduced pressure. The obtained solid residue was recrystallized from acetonitrile, whereat there were obtained 610 mg (60%) of 2-hydroxy-3,5-diisopropyl benzonitrile.

후처리

  1. extractionAfter extraction with ethyl acetate
  2. washwashing with a saturated sodium chloride solution and 2N hydrochloric acid
  3. customthe organic layer was dried
  4. customevaporated under reduced pressure
  5. customThe obtained solid residue was recrystallized from acetonitrile, whereat there

출처 및 근거

ORD 기록
ord-42dfc3c4923e4cdcac231d2c808bdb1e
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07208518B2

반응 노트

불러오는 중…