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Phosphorus oxychloride → HCID 19043054、化合物

HRID 1683195
ノート
印刷プレビュー

反応式

HRID 1683195 の反応式
C(NCC[C:6]1[C:11]2[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][C:10]=2[CH:9]=[CH:8][CH:7]=1)=O.P(Cl)(Cl)(Cl)=O.[CH3:22][O:23][C:24]1[CH:29]=[CH:28][C:27]([S:30]([CH2:33][CH3:34])(=[O:32])=[O:31])=[CH:26][C:25]=1[C:35]1[NH:36][CH:37]=[CH:38][CH:39]=1.[BH4-].[Na+]>ClCCCl.O.CO>[C:6]1([N:36]([CH2:37][C:37]2[NH:36][C:35]([C:25]3[CH:26]=[C:27]([S:30]([CH2:33][CH3:34])(=[O:31])=[O:32])[CH:28]=[CH:29][C:24]=3[O:23][CH3:22])=[CH:39][CH:38]=2)[CH2:35][CH3:25])[C:11]2[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][C:10]=2[CH:9]=[CH:8][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 24813Phosphorus oxychlorideHCID 4311764Sodium borohydrideHCID 139003532-[5-(Ethanesulfonyl)-2-methoxyphenyl]-1H-pyrroleHCID 86750935HCID 86750935、化合物

生成物 1

HCID 19043054HCID 19043054、化合物収率 207.2%

試薬・触媒・溶媒 3

HCID 11
1,2-Dichloroethane
溶媒
2 回
HCID 887Methanol溶媒
HCID 962Water溶媒2 回

実験手順

N-Formyl-N-(benzocycloheptan-1-yl)ethylamine (0.39 g, 1.81 mmol) was treated with phosphorus oxychloride (0.17 ml, 1.81 mmol) at room temperature under argon. After 30 minutes, 1,2-dichloroethane (1.2 ml) was added at 0° C. followed by a solution of 2-(2-methoxy-5-ethylsulfonylphenyl)-1H-pyrrole (0.4 g, 1.51 mmol) in 1,2-dichloroethane (4 ml). The mixture was allowed to warm to room temperature and stirred for 16 h at 25° C. and then for 6 h at 40° C. Sodium borohydride (0.55 g, 14.5 mmol) was then added at 0° C., and the reaction mixture was warmed to room temperature and stirred for 3 h. Water (2.4 ml) and then methanol (2.4 ml) were added dropwise. More water (30 ml) was added and the borane complex was extracted with dichloromethane (3×30 ml). The combined organics were dried (Na2SO4) and evaporated to an oil which was then treated with methanol (4.8 ml) and conc. HCl (2.4 ml) at room temperature for 16 h. The mixture was diluted with water (25 ml) and basified with 40% aqueous NaOH. Extraction into dichloromethane (3×30 ml), followed by drying (Na2SO4) and evaporation of the organic extracts gave an orange oil (0.73 g). The crude material was purified by chromatography on silica eluting with ethyl acetate (20-50%)--hexane, to give the title compound as an orange oil (0.31 g, 44%)

後処理

  1. waitfor 6 h at 40° C
  2. temperaturethe reaction mixture was warmed to room temperature
  3. stirringstirred for 3 h
  4. extractionthe borane complex was extracted with dichloromethane (3×30 ml)
  5. dry with materialThe combined organics were dried (Na2SO4)
  6. customevaporated to an oil which
  7. additionwas then treated with methanol (4.8 ml) and conc. HCl (2.4 ml) at room temperature for 16 h
  8. additionThe mixture was diluted with water (25 ml)
  9. extractionExtraction into dichloromethane (3×30 ml)
  10. customby drying
  11. custom(Na2SO4) and evaporation of the organic extracts

出典と根拠

ORDレコード
ord-edaa01d2f61948dd80950de85b8fcbc5
出典データセット
uspto-grants-1997_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05637609

反応ノート

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