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Hydrochloric Acid → 1,3-Dichloro-7-methoxyisoquinoline

HRID 1472723
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인쇄 미리보기

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HRID 1472723 반응식
O/[N:2]=[C:3]1/[C:4](=O)[C:5]2[C:10]([CH2:11]/1)=[CH:9][CH:8]=[C:7]([O:12][CH3:13])[CH:6]=2.P(Cl)(Cl)(Cl)(Cl)[Cl:16].[ClH:21]>O=P(Cl)(Cl)Cl>[Cl:21][C:4]1[C:5]2[C:10](=[CH:9][CH:8]=[C:7]([O:12][CH3:13])[CH:6]=2)[CH:11]=[C:3]([Cl:16])[N:2]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 24819Phosphorus pentachlorideHCID 6415827HCID 6415827, 화합물

생성물 1

HCID 716915371,3-Dichloro-7-methoxyisoquinoline수율 85%

시약·촉매·용매 1

HCID 24813Phosphorus oxychloride용매

반응 조건

온도
30 °C

실험 절차

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

To a suspension of (E)-2-(hydroxyimino)-6-methoxy-2,3-dihydro-1H-inden-1-one (3.60 g, 20.0 mmol) in POCl3 (120 mL), PCl5 (6.50 g, 31.3 mmol) was added at 0° C., then HCl gas was induced until the solution was saturated. The reaction mixture was stirred at 30° C. for 2 hours. The solvent was removed in vacuo and ice water was added to the residue. The precipitate was collected by filtration, washed with water (30 mL), and dried under high vacuum to give the product (4.50 g, yield 85%) as a solid.

후처리

  1. additionwas added at 0° C.
  2. customThe solvent was removed in vacuo and ice water
  3. additionwas added to the residue
  4. filtrationThe precipitate was collected by filtration
  5. washwashed with water (30 mL)
  6. customdried under high vacuum

출처 및 근거

ORD 기록
ord-8fc36b4771ce4bb8bdd90303b078d19f
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09012646B2

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