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

HRID 911351노트

반응식

HRID 911351 반응식
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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-8a89cab03fa345eca7dc8210d70144fa
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08022062B2

반응 노트

불러오는 중…