1,1-Bis(methylthio)-2-nitroethylene → 3-(3-pyridylmethyl)2-nitromethylenetetrahydro-2H-1,3-thiazine

HRID 1079419ノート

反応式

HRID 1079419 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([CH2:7][NH:8][CH2:9][CH2:10][CH2:11][SH:12])[CH:2]=1.[N+:13]([CH:16]=[C:17](SC)SC)([O-:15])=[O:14]>C(O)C>[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([CH2:7][N:8]2[CH2:9][CH2:10][CH2:11][S:12][C:17]2=[CH:16][N+:13]([O-:15])=[O:14])[CH:2]=1

参加物

4

反応物 2

HCID 836231,1-Bis(methylthio)-2-nitroethyleneHCID 13752794N-(3-pyridylmethyl)3-aminopropanethiol

生成物 1

HCID 539788653-(3-pyridylmethyl)2-nitromethylenetetrahydro-2H-1,3-thiazine収率 48.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of N-(3-pyridylmethyl)3-aminopropanethiol (1.8 g), 1-nitro-2,2-bis(methylthio)ethylene (1.7 g) and ethanol (40 ml) was heated under reflux for 5 hours under a nitrogen stream. After the reaction, about 2/3 by volume of ethanol was distilled off under reduced pressure. Ether was added little by little to the reaction mixture to precipitate crystals. The crystals were collected by filtration, and washed with a mixture of ethanol and there to give the desired 3-(3-pyridylmethyl)2-nitromethylenetetrahydro-2H-1,3-thiazine (1.2 g).

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 5 hours under a nitrogen stream
  3. customAfter the reaction
  4. distillationabout 2/3 by volume of ethanol was distilled off under reduced pressure
  5. additionEther was added little by little to the reaction mixture
  6. customto precipitate crystals
  7. filtrationThe crystals were collected by filtration
  8. washwashed with a mixture of ethanol

出典と根拠

ORDレコード
ord-ba88d1ced1234a648c3c6d8d3bea584c
出典データセット
uspto-grants-1996_12
特許番号
US05580889

反応ノート

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