Phosphorus oxychloride → HCID 5156493、化合物

HRID 968490ノート

反応式

HRID 968490 の反応式
[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

参加物

5

反応物 2

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

生成物 1

HCID 5156493HCID 5156493、化合物収率 98%

試薬・触媒・溶媒 2

HCID 66133Benzyl triethylammonium chloride触媒HCID 6342Acetonitrile溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-63c517d4ac0a4d029f4ce84c232c7aa7
出典データセット
uspto-grants-2007_12
特許番号
US07304052B2

反応ノート

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