Formaldehyde → N,S-Dimethyl-S-(4-nitrophenyl)sulfoximine

HRID 1891081노트

반응식

HRID 1891081 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([S:10]([CH3:13])(=[NH:12])=[O:11])=[CH:6][CH:5]=1)([O-:3])=[O:2].[CH2:14]=O>C(O)=O>[CH3:14][N:12]=[S:10]([CH3:13])([C:7]1[CH:6]=[CH:5][C:4]([N+:1]([O-:3])=[O:2])=[CH:9][CH:8]=1)=[O:11]

참가 물질

4

반응물 2

HCID 712FormaldehydeHCID 12463933S-Methyl-S-(4-nitrophenyl)sulfoximine

생성물 1

HCID 12463940N,S-Dimethyl-S-(4-nitrophenyl)sulfoximine

시약·촉매·용매 1

HCID 284Formic Acid용매

반응 조건

온도
100 °C

실험 절차

500 mg (2.5 mmol) of (RS)—S-(4-nitrophenyl)-S-methyl sulfoximide in 4 ml of formaldehyde (aqueous, 37%) and 20 ml of formic acid (98-100%) are stirred in an open flask at 100° C. After 22 hours, the solvent is evaporated, mixed again with 4 ml of formaldehyde (aqueous, 37%) and 20 ml of formic acid (98-100%) and stirred for another 22 hours at 100° C. Residue from the solvent is drawn off in a rotary evaporator. The remaining residue is dissolved with 2N HCl and extracted from DCM. The aqueous phase is made basic with NaHCO3 and extracted from DCM. The combined organic phases are dried (Na2SO4), filtered and concentrated by evaporation. 448 mg (2.1 mmol, corresponding to 85% of theory) of the product is obtained.

후처리

  1. customthe solvent is evaporated
  2. additionmixed again with 4 ml of formaldehyde (aqueous, 37%) and 20 ml of formic acid (98-100%)
  3. customResidue from the solvent is drawn off in a rotary evaporator
  4. dissolutionThe remaining residue is dissolved with 2N HCl
  5. extractionextracted from DCM
  6. extractionextracted from DCM
  7. dry with materialThe combined organic phases are dried (Na2SO4)
  8. filtrationfiltered
  9. concentrationconcentrated by evaporation
  10. custom448 mg (2.1 mmol, corresponding to 85% of theory) of the product is obtained

출처 및 근거

ORD 기록
ord-f7b9e699f289418ab8ab91018c1350d0
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08507510B2

반응 노트

불러오는 중…