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

HRID 4805

反応式

HRID 4805 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-6e0e6792bd184b57bc64b7b90119b242
出典データセット
uspto-grants-1988_02
特許番号
US04727152

関連ノート

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