5-chloro-N-methylpyridin-2-amine → 1,1-bis(phenylsulphonyl)-2-[N-(5-chloropyrid-2-yl)-N-methylamino]ethene

HRID 542893

반응식

HRID 542893 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([NH:8][CH3:9])=[N:6][CH:7]=1.C(O[CH:13]=[C:14]([S:24]([C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)(=[O:26])=[O:25])[S:15]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)(=[O:17])=[O:16])C>Cl.C1(C)C=CC=CC=1.N12CCCC1=NCCC2>[C:27]1([S:24]([C:14]([S:15]([C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=2)(=[O:17])=[O:16])=[CH:13][N:8]([C:5]2[CH:4]=[CH:3][C:2]([Cl:1])=[CH:7][N:6]=2)[CH3:9])(=[O:25])=[O:26])[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=1

참가 물질

6

반응물 2

HCID 38370245-chloro-N-methylpyridin-2-amineHCID 124009381,1-Bis(phenylsulphonyl)-2-ethoxyethene

생성물 1

HCID 202074401,1-bis(phenylsulphonyl)-2-[N-(5-chloropyrid-2-yl)-N-methylamino]ethene

시약·촉매·용매 3

HCID 313Hydrochloric Acid촉매HCID 763491,5-Diazabicyclo(4.3.0)non-5-ene촉매HCID 1140Toluene용매

실험 절차

A mixture of 5-chloro-2-(methylamino)pyridine (0.41 g), 2-ethoxy-1,1-bis(phenylsulphonyl)ethene and concentrated hydrochloric acid (1 drop) in toluene (20 ml) was heated at reflux for 4 hours and then the mixture was treated with 1,5-diazabicyclo[4.3.0]-non-5-ene (3 drops) and heated at reflux for 18 hours. The reaction mixture was cooled and concentrated in vacuo to give an oil which was triturated with ethanol to give a brown solid which was recrystallised from toluene to give 1,1-bis(phenylsulphonyl)-2-[N-(5-chloropyrid-2-yl)-N-methylamino]ethene (0.2 g), mp. 205°-206° C.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 4 hours
  3. temperatureheated
  4. temperatureat reflux for 18 hours
  5. temperatureThe reaction mixture was cooled
  6. concentrationconcentrated in vacuo
  7. customto give an oil which
  8. customwas triturated with ethanol
  9. customto give a brown solid which
  10. customwas recrystallised from toluene

출처 및 근거

ORD 기록
ord-b3a9fe616479454fa1f454e11bde5baa
출처 데이터셋
uspto-grants-1987_04
특허 번호
US04659727

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