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Pyridine → 6-Decyl-3-methylthio-2-(trifluoromethanesulfonyloxy)naphthalene

HRID 1476373
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HRID 1476373 반응식
FC(F)(F)S([O:6][S:7]([C:10]([F:13])([F:12])[F:11])(=[O:9])=[O:8])(=O)=O.ClCCl.[CH2:19]([C:29]1[CH:30]=[C:31]2[C:36](=[CH:37][CH:38]=1)[CH:35]=[C:34](O)[C:33]([S:40][CH3:41])=[CH:32]2)[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28].N1C=CC=CC=1>O.Cl>[CH2:19]([C:29]1[CH:30]=[C:31]2[C:36](=[CH:37][CH:38]=1)[CH:35]=[C:34]([O:6][S:7]([C:10]([F:11])([F:12])[F:13])(=[O:8])=[O:9])[C:33]([S:40][CH3:41])=[CH:32]2)[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 1049PyridineHCID 6344DichloromethaneHCID 67749Trifluoromethanesulfonic anhydrideHCID 867043886-Decyl-3-methylthio-2-hydroxynaphthalene

생성물 1

HCID 867043896-Decyl-3-methylthio-2-(trifluoromethanesulfonyloxy)naphthalene수율 105.7%

시약·촉매·용매 2

HCID 313
Hydrochloric Acid
용매
HCID 962Water용매

실험 절차

Trifluoromethanesulfonic anhydride (3 ml, 15 mmol) was added to a dichloromethane (50 ml) solution of the obtained 6-decyl-3-methylthio-2-hydroxynaphthalene (3.63 g, 10 mmol) and pyridine (2.5 ml, 30 mmol) at 0° C. This solution was stirred at room temperature for 25 minutes. Then, the mixture was diluted with water (20 ml), and hydrochloric acid (4 M, 20 ml) was added. The mixture was extracted with dichloromethane (30 ml×3). The organic phases obtained by repeating the extraction three times were collected, washed with saturated saline water (30 ml×3), dried with MgSO4, and condensed to obtain 6-decyl-3-methylthio-2-(trifluoromethanesulfonyloxy)naphthalene (compound (4)-81) (4.89 g, 99%).

후처리

  1. additionwas added
  2. extractionThe mixture was extracted with dichloromethane (30 ml×3)
  3. customThe organic phases obtained
  4. extractionthe extraction three times
  5. customwere collected
  6. washwashed with saturated saline water (30 ml×3)
  7. dry with materialdried with MgSO4, and condensed

출처 및 근거

ORD 기록
ord-ed4e1ddcc0824711a242da0d5b994ca5
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09018630B2

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