Phosphorus oxide (P4O10) → 6,7-Dichloro-3,4-dihydro-2H-isoquinolin-1-one

HRID 1843977노트

반응식

HRID 1843977 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:13]=[CH:14][C:15]=1[Cl:16])[CH2:5][CH2:6][NH:7][C:8](=O)[O:9]CC.O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>O=P(Cl)(Cl)Cl>[Cl:1][C:2]1[CH:3]=[C:4]2[C:13](=[CH:14][C:15]=1[Cl:16])[C:8](=[O:9])[NH:7][CH2:6][CH2:5]2

참가 물질

4

반응물 2

HCID 14812Phosphorus oxide (P4O10)HCID 66802053HCID 66802053, 화합물

생성물 1

HCID 141771016,7-Dichloro-3,4-dihydro-2H-isoquinolin-1-one수율 20.3%

시약·촉매·용매 1

HCID 24813Phosphorus oxychloride용매

실험 절차

Using an analogous procedure and workup as described for the preparation of intermediate I-1d above, ethyl 3,4-dichlorophenethylcarbamate (I-55c: 6 g, 22.989 mmol) in POCl3 (60 mL) was reacted with P2O5 (6.52 g, 45.977 mmol) at 120° C. for 1 hour to afford the crude product. Purification by column chromatography on silica gel (30% ethylacetate in hexane) afforded 1.01 g of the product. LCMS: 53.61%, m/z=216.0 (M+1)

후처리

  1. customworkup as described for the preparation of intermediate I-1d above
  2. customto afford the crude product
  3. customPurification by column chromatography on silica gel (30% ethylacetate in hexane)

출처 및 근거

ORD 기록
ord-e46051135ec24ace956c5cd3c6f29d58
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08946260B2

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