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

HRID 1843928노트

반응식

HRID 1843928 반응식
C([O:3][C:4](=O)[NH:5][CH2:6][CH2:7][C:8]1[CH:13]=[CH:12][C:11]([Cl:14])=[C:10]([Cl:15])[CH:9]=1)C.O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>O=P(Cl)(Cl)Cl>[Cl:15][C:10]1[CH:9]=[C:8]2[C:13](=[CH:12][C:11]=1[Cl:14])[C:4](=[O:3])[NH:5][CH2:6][CH2:7]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 12.1%

시약·촉매·용매 1

HCID 24813Phosphorus oxychloride용매

실험 절차

Using an analogous reaction procedure and workup as described in Example 1, [2-(3,4-dichloro-phenyl)-ethyl]-carbamic acid ethyl ester (I-41c: 3.5 g, 13.409 mmol) in POCl3 (35 mL) was reacted with P2O5 (3.80 g, 26.819 mmol) at 120° C. for 1 hour to afford the crude product. Purification by column chromatography on silica gel (30% ethylacetate in hexane) afforded 0.350 g of the crude product which was used in the next step without further purification.

후처리

  1. customan analogous reaction procedure
  2. customto afford the crude product
  3. customPurification by column chromatography on silica gel (30% ethylacetate in hexane)

출처 및 근거

ORD 기록
ord-df0e10cf43334a828777bf8514179fe7
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08946260B2

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