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Trifluoroacetic acid → (RS) 7-(Methylthio)-1,2,3,4,10,10a-hexahydropyrazino[1,2-a]indole Fumarate

HRID 857467
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HRID 857467 반응식
FC(F)(F)C(O)=O.C(OC([N:15]1[CH2:29][CH2:28][N:18]2[C:19]3[CH:20]=[C:21]([S:26][CH3:27])[CH:22]=[CH:23][C:24]=3[CH2:25][CH:17]2[CH2:16]1)=O)(C)(C)C.C(=O)([O-])O.[Na+].[C:35]([OH:42])(=[O:41])/[CH:36]=[CH:37]/[C:38]([OH:40])=[O:39]>ClCCl.CC(O)C>[C:35]([OH:42])(=[O:41])/[CH:36]=[CH:37]/[C:38]([OH:40])=[O:39].[CH3:27][S:26][C:21]1[CH:22]=[CH:23][C:24]2[CH2:25][CH:17]3[CH2:16][NH:15][CH2:29][CH2:28][N:18]3[C:19]=2[CH:20]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6422Trifluoroacetic acidHCID 444972Fumaric AcidHCID 516892Sodium BicarbonateHCID 218687642-Tert-butoxycarbonyl-7-(methylthio)-1,2,3,4,10,10a-hexahydropyrazino[1,2-a]indole

생성물 1

HCID 21868744(RS) 7-(Methylthio)-1,2,3,4,10,10a-hexahydropyrazino[1,2-a]indole Fumarate수율 54%

시약·촉매·용매 2

HCID 3776
Isopropanol
용매
HCID 6344Dichloromethane용매

실험 절차

Trifluoroacetic acid (1 mL) was added to a stirred solution of 2-tert-butoxycarbonyl-7-(methylthio)-1,2,3,4,10,10a-hexahydropyrazino[1,2-a]indole (70 mg, 0.21 mmol) in dichloromethane. (5 mL) at room temperature under Ar. The reaction was stirred at room temperature for 1 h then poured into saturated aqueous sodium hydrogen carbonate solution (50 mL) and extracted with dichloromethane (3×30 mL). The combined organic extracts, were washed with brine (1×30 mL), dried (magnesium sulfate), filtered and the solvent removed under vacuum to leave a crude oil. The oil was dissolved in 2-propanol (5 mL) and heated to reflux. Fumaric acid (1 eq) was added and the solution was cooled to room temperature. The emerging precipitate was filtered, washed with ether and dried to give the product as a white solid (40 mg, 54%). mp 196–198° C. Found: C, 56.50; H, 5.89; N, 8.15%. C12H16N2S. 1.1 C4H4O4 requires: C, 56.60; H, 5.91; N, 8.05%. IR νmax (Nujol)/cm−1 3595, 3188, 2925, 2854, 2457, 1696, 1585, 1485, 1486, 1461, 1402, 1377, 1345, 1317, 1279, 1230, 1179, 1154, 1129, 1066, 1058, 1005, 996, 972, 919, 987, 868, 835, 797, 722, 644, 606, 547 and 482: NMR δH (400 MHz; DMSO-d6) 6.99 (1H, d, J 7.5 Hz), 6.52 (2H, s), 6.47–6.51 (2H, m), 3.69–3.72 (1H, m), 3.50–3.62 (2H, m), 3.05–3.20 (3H, m), 2.91–3.02 (2H, m), 2.65–2.80 (2H, m), 2.43 (3H, s).

후처리

  1. customat room temperature
  2. extractionextracted with dichloromethane (3×30 mL)
  3. washThe combined organic extracts, were washed with brine (1×30 mL)
  4. dry with materialdried (magnesium sulfate)
  5. filtrationfiltered
  6. customthe solvent removed under vacuum
  7. customto leave a crude oil
  8. temperatureheated to reflux
  9. temperaturethe solution was cooled to room temperature
  10. filtrationThe emerging precipitate was filtered
  11. washwashed with ether
  12. customdried

출처 및 근거

ORD 기록
ord-cc508cc762f04b948c30cd2018c7a3fe
출처 데이터셋
uspto-grants-2006_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07145009B2

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