2,4-Bis(trifluoromethyl)benzaldehyde → (NE)-N-[[2,4-bis(trifluoromethyl)phenyl]methylidene]-2-methylpropane-2-sulfinamide

HRID 12601

반응식

HRID 12601 반응식
[F:1][C:2]([F:16])([F:15])[C:3]1[CH:10]=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:8]=[CH:7][C:4]=1[CH:5]=O.[C:17]([S:21]([NH2:23])=[O:22])([CH3:20])([CH3:19])[CH3:18]>C(Cl)Cl.O.[O-]S([O-])(=O)=O.[Cu+2]>[F:1][C:2]([F:16])([F:15])[C:3]1[CH:10]=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:8]=[CH:7][C:4]=1/[CH:5]=[N:23]/[S:21]([C:17]([CH3:20])([CH3:19])[CH3:18])=[O:22]

참가 물질

6

반응물 2

HCID 27360952,4-Bis(trifluoromethyl)benzaldehydeHCID 3382465Tert-Butanesulfinamide

생성물 1

HCID 178455562(NE)-N-[[2,4-bis(trifluoromethyl)phenyl]methylidene]-2-methylpropane-2-sulfinamide

시약·촉매·용매 3

HCID 24462Copper Sulfate촉매HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

A mixture of 2,4-bis trifluoromethyl benzaldehyde (10.0 g, 41.3 mmol), tert butyl sulfinamide (4.5 g, 37.2 mmol) and anhydrous CuSO4 (13.1 g, 82.6 mmol) in DCM (100 ml) was stirred at room temperature overnight. The fine suspension was diluted with water and extracted with DCM. The extracts were washed with water, dried (MgSO4) and evaporated in vacuo to afford the desired N-{(1E)-[2,4-bis(trifluoro methyl)phenyl]methylene}-2-methylpropane-2-sulfinamide as an off white solid (7.62 g, 53%), with no further purification. 1H NMR δ (ppm)(CDCl3): 8.99 (1 H, d, J=1.9 Hz), 8.35 (1 H, d, J=8.2 Hz), 8.02 (1 H, s), 7.92 (1 H, d, J=8.2 Hz), 1.28 (9 H, d, J=4.6 Hz); m/z (ES+) 346 (MH+).

후처리

  1. extractionextracted with DCM
  2. washThe extracts were washed with water
  3. dry with materialdried (MgSO4)
  4. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-d8a15633b09740b3a83773b2d22693a7
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728022B2

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