Phosphorus sulfide (P2S5) → 2-(chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f]-1,4-oxazepine-5(4H)thione

HRID 4805

반응식

HRID 4805 반응식
Cl.[Cl:2][CH2:3][CH2:4][CH:5]1[CH2:11][N:10]([CH3:12])[C:9](=O)[C:8]2[CH:14]=[CH:15][CH:16]=[N:17][C:7]=2[O:6]1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:19]>C(Cl)(Cl)Cl>[Cl:2][CH2:3][CH2:4][CH:5]1[CH2:11][N:10]([CH3:12])[C:9](=[S:19])[C:8]2[CH:14]=[CH:15][CH:16]=[N:17][C:7]=2[O:6]1

참가 물질

4

반응물 2

HCID 14817Phosphorus sulfide (P2S5)HCID 137264372-(2-chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]oxazepin-5(4H)one hydrochloride

생성물 1

HCID 137264422-(chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f]-1,4-oxazepine-5(4H)thione

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

To a solution of 59 g (0.25 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]oxazepin-5(4H)one hydrochloride in 1500 ml of chloroform was added 41.5 g (0.19 mole) of phosphorus pentasulfide and the mixture was heated to reflux for 18 hr. The mixture was filtered and the filtrate was extracted with dilute sodium hydroxide. The chloroform layer was concentrated and the residue was dissolved in 250 ml of boiling isopropyl alcohol. On cooling, 28 g (44%) of yellow solid precipitated. A portion was recrystallized from isopropyl alcohol, m.p. 134°-136° C.

후처리

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 18 hr
  3. filtrationThe mixture was filtered
  4. extractionthe filtrate was extracted with dilute sodium hydroxide
  5. concentrationThe chloroform layer was concentrated
  6. dissolutionthe residue was dissolved in 250 ml of boiling isopropyl alcohol
  7. temperatureOn cooling
  8. custom28 g (44%) of yellow solid precipitated
  9. customA portion was recrystallized from isopropyl alcohol, m.p. 134°-136° C.

출처 및 근거

ORD 기록
ord-6e0e6792bd184b57bc64b7b90119b242
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04727152

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