Water → HCID 18509409, 화합물

HRID 1356810노트

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HRID 1356810 반응식
[CH3:1][C:2]([CH3:23])([CH3:22])[C:3]#[C:4]/[CH:5]=[CH:6]/[CH2:7][N:8]([CH2:10][C:11]1[CH:12]=[C:13]([C:18](O)([CH3:20])[CH3:19])[CH:14]=[CH:15][C:16]=1[CH3:17])[CH3:9].P(Cl)(Cl)(Cl)=O.O.[OH-].[Na+]>N1C=CC=CC=1>[CH3:1][C:2]([CH3:23])([CH3:22])[C:3]#[C:4]/[CH:5]=[CH:6]/[CH2:7][N:8]([CH2:10][C:11]1[CH:12]=[C:13]([C:18]([CH3:20])=[CH2:19])[CH:14]=[CH:15][C:16]=1[CH3:17])[CH3:9]

참가 물질

6

반응물 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 24813Phosphorus oxychlorideHCID 18509459HCID 18509459, 화합물

생성물 1

HCID 18509409HCID 18509409, 화합물수율 85.7%

시약·촉매·용매 1

HCID 1049Pyridine용매

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온도
135 °C

실험 절차

Compound 33 (520 mg; 1.66 mmol) was dissolved in pyridine (6 ml), and phosphorus oxychloride (1.27 g; 8.3 mmol) was added thereto. The mixture was stirred for 1 hour at 130-140° C., and then cooled. The reaction mixture was poured into water, and alkalinized with sodium hydroxide pellet. The mixture was extracted with ether (120 ml), and dried over magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=20:1), to thereby yield 420 mg of the target compound (yield: 85.7%).

후처리

  1. temperaturecooled
  2. extractionThe mixture was extracted with ether (120 ml)
  3. dry with materialdried over magnesium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customthe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=20:1)

출처 및 근거

ORD 기록
ord-b8a87f0af27742d1bf7aa592ca0f257b
출처 데이터셋
uspto-grants-2003_07
특허 번호
US06586633B1

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