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

HRID 857467
ノート
印刷プレビュー

反応式

HRID 857467 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 3776
Isopropanol
溶媒
HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-cc508cc762f04b948c30cd2018c7a3fe
出典データセット
uspto-grants-2006_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07145009B2

反応ノート

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