Phosphorus oxychloride → HCID 5156493, 화합물

HRID 968490노트

반응식

HRID 968490 반응식
[N+:1]([C:4]1[C:5](=O)[NH:6][C:7]2[CH2:8][CH2:9][CH2:10][CH2:11][C:12]=2[CH:13]=1)([O-:3])=[O:2].P(Cl)(Cl)([Cl:17])=O>CC[N+](CC1C=CC=CC=1)(CC)CC.[Cl-].C(#N)C>[Cl:17][C:5]1[C:4]([N+:1]([O-:3])=[O:2])=[CH:13][C:12]2[CH2:11][CH2:10][CH2:9][CH2:8][C:7]=2[N:6]=1

참가 물질

5

반응물 2

HCID 24813Phosphorus oxychlorideHCID 33236953-Nitro-1,2,5,6,7,8-hexahydroquinolin-2-one

생성물 1

HCID 5156493HCID 5156493, 화합물수율 98%

시약·촉매·용매 2

HCID 66133Benzyl triethylammonium chloride촉매HCID 6342Acetonitrile용매

실험 절차

A solution of intermediate (8) (0.072 mol) and BTEAC (0.0362 mol) in ACN (150 ml) was stirred at room temperature. Phosphoric trichloride (0.222 mol) was added dropwise. The mixture was stirred and refluxed for 8 hours. The solvent was evaporated till dryness. The residue was poured out into water and NH4OH. The mixture was extracted with DCM. The organic layer was separated, dried, filtered and the solvent was evaporated, yielding 15 g of 2-chloro-5,6,7,8-tetrahydro-3-nitroquinoline (intermediate 9).

후처리

  1. temperaturerefluxed for 8 hours
  2. customThe solvent was evaporated till dryness
  3. additionThe residue was poured out into water and NH4OH
  4. extractionThe mixture was extracted with DCM
  5. customThe organic layer was separated
  6. customdried
  7. filtrationfiltered
  8. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-63c517d4ac0a4d029f4ce84c232c7aa7
출처 데이터셋
uspto-grants-2007_12
특허 번호
US07304052B2

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