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Phosphorus pentachloride → 5-Isoquinolinesulfonyl chloride

HRID 1977944
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HRID 1977944 반응식
[CH:1]1[C:10]2[CH:9]=[CH:8][CH:7]=[C:6]([S:11]([OH:14])(=O)=[O:12])[C:5]=2[CH:4]=[CH:3][N:2]=1.P(Cl)(Cl)(Cl)(Cl)[Cl:16]>P(Cl)(Cl)(Cl)=O.C(Cl)(Cl)Cl>[CH:1]1[C:10]2[CH:9]=[CH:8][CH:7]=[C:6]([S:11]([Cl:16])(=[O:14])=[O:12])[C:5]=2[CH:4]=[CH:3][N:2]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 24819Phosphorus pentachlorideHCID 2415995-Isoquinolinesulfonic acid

생성물 1

HCID 33716555-Isoquinolinesulfonyl chloride수율 96.6%

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 24813Phosphorus oxychloride용매

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온도
120 °C

실험 절차

A mixture of 5-isoquinolinesulfonic acid (4.18 g, 20 mmol), and phosphorus pentachloride (6.24 g, 30 mmol) in phosphorus oxychloride (20 mL) was heated at 120 ° C. for two days. The reaction mixture was cooled to room temperature and diluted with dry chloroform (60 mL). The white precipitate was collected, washed with dry chloroform, and dried under high vacuum to give the title compound as a white solid (4.40 g, 83%) which was used for next step without further purification. 1H-NMR (300 MHz, CDCl3)δ9.95 (s, 1H), 9.16 (d, J=6.8 Hz, 1H), 8.74 (d, J=6.8 Hz, 1H), 8.52 (t, J=7.0 Hz, 2H), 7.99 (t, J=7.3 Hz, 1H).

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. customThe white precipitate was collected
  3. washwashed with dry chloroform
  4. customdried under high vacuum

출처 및 근거

ORD 기록
ord-ef11fe6cfad8490b90fbc1e151fc6c83
출처 데이터셋
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06235778B1

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