Hydrochloric Acid → N-[(5-Phenylthiophen-2-yl)-methylene]-2-methylpropanesulfinamide

HRID 911351ノート

反応式

HRID 911351 の反応式
C1(C2SC(C(N)C)=CC=2)C=CC=CC=1.Cl.O1CCOCC1.[C:22]1([C:28]2[S:32][C:31]([CH:33]([NH:35][S:36]([CH2:38][CH:39]([CH3:41])[CH3:40])=[O:37])C)=[CH:30][CH:29]=2)[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1>CO>[C:22]1([C:28]2[S:32][C:31]([CH:33]=[N:35][S:36]([CH2:38][CH:39]([CH3:41])[CH3:40])=[O:37])=[CH:30][CH:29]=2)[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 30320191-(5-Phenylthiophen-2-yl)ethan-1-amineHCID 66706418N-[1-(5-phenylthiophen-2-yl)ethyl]-2-methylpropanesulfinamide

生成物 1

HCID 66706412N-[(5-Phenylthiophen-2-yl)-methylene]-2-methylpropanesulfinamide収率 77%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

1-(5-Phenyl-thiophen-2-yl)ethylamine (Isomer 2, Preparation 171) Add 4N hydrogen chloride in dioxane (1.112 mL, 4.449 mmol) to a stirred solution of N-[1-(5-phenylthiophen-2-yl)ethyl]-2-methylpropanesulfinamide (Isomer 2) (684 mg, 2.225 mmol) in methanol (10 mL) at room temperature. Stir for 2 h and remove the solvent in vacuo to obtain a solid that was washed with ethyl ether. Dissolve the solid in DCM and wash with saturated aqueous NaHCO3. Dry the organic phase over Na2SO4, filter and concentrate in vacuo to obtain the desired intermediate (347 mg, 77% yield).

後処理

  1. customremove the solvent in vacuo
  2. customto obtain a solid
  3. washthat was washed with ethyl ether
  4. dissolutionDissolve the solid in DCM
  5. washwash with saturated aqueous NaHCO3
  6. dry with materialDry the organic phase over Na2SO4
  7. filtrationfilter
  8. concentrationconcentrate in vacuo

出典と根拠

ORDレコード
ord-8a89cab03fa345eca7dc8210d70144fa
出典データセット
uspto-grants-2011_09
特許番号
US08022062B2

反応ノート

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