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Tert-Butanesulfinamide → HCID 87333909, 화합물

HRID 1698508
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HRID 1698508 반응식
[CH2:1]([S:4]([C:7]1[CH:14]=[CH:13][C:10]([CH:11]=O)=[CH:9][CH:8]=1)(=[O:6])=[O:5])[CH2:2][CH3:3].[C:15]([S:19]([NH2:21])=[O:20])([CH3:18])([CH3:17])[CH3:16]>[O-]CC.[Ti+5].[O-]CC.[O-]CC.[O-]CC.[O-]CC.C1COCC1>[CH3:16][C:15]([S:19](/[N:21]=[CH:11]/[C:10]1[CH:13]=[CH:14][C:7]([S:4]([CH2:1][CH2:2][CH3:3])(=[O:6])=[O:5])=[CH:8][CH:9]=1)=[O:20])([CH3:18])[CH3:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 3382465Tert-ButanesulfinamideHCID 204932624-(Propane-1-sulfonyl)-benzaldehyde

생성물 1

HCID 87333909HCID 87333909, 화합물

시약·촉매·용매 2

HCID 178468024HCID 178468024, 화합물촉매HCID 8028Tetrahydrofuran용매

실험 절차

4-(Propylsulphonyl)benzaldehyde (1.81 g, 8.53 mmol, prepared as described in Example 47a, tert-butyl sulphinamide (1.55 g, 12.8 mmol), titanium(V) ethoxide (3.58 mL, 17.1 mmol) and THF (50 mL) were heated at reflux for 3 h then stirred at room temperature overnight. The reaction mixture was quenched with water (200 mL) before addition of ethyl acetate (200 mL). Celite was added and the mixture stirred for 15 min before being filtered. The phases were separated and the organic extract dried (MgSO4) and concentrated. The yield of the title compound was assumed to be quantitative and the material was used without further purification. m/z (ES+) 316 (M+H).

후처리

  1. temperaturewere heated
  2. temperatureat reflux for 3 h
  3. customThe reaction mixture was quenched with water (200 mL) before addition of ethyl acetate (200 mL)
  4. additionCelite was added
  5. stirringthe mixture stirred for 15 min
  6. filtrationbefore being filtered
  7. customThe phases were separated
  8. extractionthe organic extract
  9. dry with materialdried (MgSO4)
  10. concentrationconcentrated
  11. customthe material was used without further purification

출처 및 근거

ORD 기록
ord-b9026cb387d2437ca7b0c276c5ec3713
출처 데이터셋
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08163956B2

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