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Phosphorus oxychloride → HCID 57842568, 화합물

HRID 735541
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HRID 735541 반응식
[CH2:1]([N:8]([CH2:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)[C:9]1[CH:10]=[C:11]2[C:16](=[C:17]([F:19])[CH:18]=1)[C:15](=O)[NH:14][CH:13]=[CH:12]2)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.P(Cl)(Cl)([Cl:30])=O>>[Cl:30][C:15]1[C:16]2[C:11](=[CH:10][C:9]([N:8]([CH2:1][C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)[CH2:21][C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)=[CH:18][C:17]=2[F:19])[CH:12]=[CH:13][N:14]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 598380236-(Dibenzylamino)-8-fluoroisoquinolin-1(2H)-one

생성물 1

HCID 57842568HCID 57842568, 화합물수율 89%

반응 조건

온도
100 °C

실험 절차

A mixture of 19D (0.622 g, 1.74 mmol) and phosphorous oxychloride (6 mL) was heated at 100° C. for 1.5 h. The reaction mixture was concentrated under reduced pressure and co-evaporated twice with toluene. Ice was added to the residue, followed by sodium hydroxide (1N solution) until the pH was basic. The mixture was extracted with methylene chloride (3×), and the combined organic layers were washed with saturated sodium bicarbonate solution and brine, dried (MgSO4), and dried in vacuo to give 19E (0.583 g, 89%) as a yellow solid.

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. additionIce was added to the residue
  3. extractionThe mixture was extracted with methylene chloride (3×)
  4. washthe combined organic layers were washed with saturated sodium bicarbonate solution and brine
  5. dry with materialdried (MgSO4)
  6. customdried in vacuo

출처 및 근거

ORD 기록
ord-ec096b94773446cfbc05c7f61c1c2903
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07592331B2

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