1,2-Dichloroethane → HCID 178423700、化合物

HRID 267915

反応式

HRID 267915 の反応式
[CH3:1][CH:2]1[NH:6][C:5](=O)[CH2:4][CH2:3]1.P(Cl)(Cl)([Cl:10])=O.[CH:13]1[C:26]2[NH:25][C:24]3[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=3)[S:18][C:17]=2[CH:16]=[CH:15][CH:14]=1.[OH-].[K+].Cl[CH2:30]CCl>>[ClH:10].[CH3:30][SH:18]1[C:17]2[C:26](=[CH:13][CH:14]=[CH:15][CH:16]=2)[NH:25][C:24]2[C:23]([C:5]3[CH2:4][CH2:3][CH:2]([CH3:1])[N:6]=3)=[CH:22][CH:21]=[CH:20][C:19]1=2

参加物

6

反応物 5

HCID 111,2-Dichloroethane2 回HCID 7108PhenothiazineHCID 14797Potassium HydroxideHCID 24813Phosphorus oxychlorideHCID 660555-Methyl-2-pyrrolidone

生成物 1

HCID 178423700HCID 178423700、化合物収率 17%

実験手順

A mixture of 5-methyl-2-pyrrolidinone (6.0 g., 0.06 mole), phosphorus oxychloride (9.2 g., 0.06 mole) in 60 ml. of 1,2-dichloroethane is refluxed for 10 min. A solution of phenothiazine (6.0 g., 0.03 mole) in 20 ml. of 1,2-dichloroethane is added at the end of the reflux period and the reaction mixture stirred and refluxed for 20 hr., and then poured onto 20 ml. of 5N potassium hydroxide and 20 g. of crushed ice. The 1,2-dichloroethane layer is separated and extracted with 30 ml. of 1.5N hydrochloric acid and 30 ml. of water removing water soluble by-product 10-[2-(5-methyl-1-pyrrolinyl)]-phenothiazine hydrochloride. After drying the 1,2-dichloroethane solution over magnesium sulfate, the 1,2-dichloroethane solution is concentrated and the solid thus obtained stirred with 40 ml. of acetone and filtered. Crystallization of the filtercake from ethanol-ether provides analytically pure 10-[5-METHYL-1-(5-METHYL-1 -PYRROLIN-2-YL]PHENOTHIAZINE HYDROCHLORIDE in a yield of 17%, m.p. 257°-264° C. (corr.).

後処理

  1. temperaturerefluxed for 20 hr
  2. addition, and then poured onto 20 ml
  3. customThe 1,2-dichloroethane layer is separated
  4. extractionextracted with 30 ml
  5. customof water removing water soluble by-product 10-[2-(5-methyl-1-pyrrolinyl)]-phenothiazine hydrochloride
  6. dry with materialAfter drying the 1,2-dichloroethane solution over magnesium sulfate
  7. concentrationthe 1,2-dichloroethane solution is concentrated
  8. customthe solid thus obtained
  9. stirringstirred with 40 ml
  10. filtrationof acetone and filtered
  11. customCrystallization of the filtercake from ethanol-ether

出典と根拠

ORDレコード
ord-be28f5f9e3d545928b4392e148b1dfae
出典データセット
uspto-grants-1976_03
特許番号
US03946004

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