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Methanol → 4-(1-(4,4,4-trifluorobutyl)-1H-benzimidazol-2-yl)[1,4]diazepane hydriodic acid salt

HRID 1584479
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HRID 1584479 반응식
C(OC([N:8]1[CH2:14][CH2:13][CH2:12][N:11]([C:15]2[N:19]([CH2:20][CH2:21][CH2:22][C:23]([F:26])([F:25])[F:24])[C:18]3[CH:27]=[CH:28][CH:29]=[CH:30][C:17]=3[N:16]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.CO.[IH:33]>C(OCC)C>[IH:33].[F:26][C:23]([F:24])([F:25])[CH2:22][CH2:21][CH2:20][N:19]1[C:18]2[CH:27]=[CH:28][CH:29]=[CH:30][C:17]=2[N:16]=[C:15]1[N:11]1[CH2:12][CH2:13][CH2:14][NH:8][CH2:9][CH2:10]1
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참가 물질

5

반응물 3

HCID 887Methanol2회HCID 24841Hydrogen iodide2회HCID 212236081-t-butoxycarbonyl-4-(1-(4,4,4-trifluorobutyl)-1H-benzimidazol-2-yl)[1,4]diazepane

생성물 1

HCID 867543574-(1-(4,4,4-trifluorobutyl)-1H-benzimidazol-2-yl)[1,4]diazepane hydriodic acid salt

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
50 °C

실험 절차

Combine 1-t-butoxycarbonyl-4-(1-(4,4,4-trifluorobutyl)-1H-benzimidazol-2-yl)[1,4]diazepane (1.80 g, 4.22 mmol) and methanol (15 mL). Cool in an ice bath. Add aqueous hydriodic acid (3.8 g, 2.23 mL, 57%, 16.9 mmol) and warm to ambient temperature. After 30 minutes, add aqueous hydriodic acid (1.12 mL) and heat to 50° C. After 2 hours, cool to ambient temperature and evaporate to remove most of the methanol to give a residue. Combine the residue and methanol (10 mL). Add diethyl ether (200 mL) and stir to give a solid. Decant the solvent, add diethyl ether (200 mL) and stir, collect the solid by filtration to give, after drying, the title compound: mp; 206-208° C.

후처리

  1. temperatureCool in an ice bath
  2. waitAfter 2 hours
  3. temperaturecool to ambient temperature
  4. customevaporate
  5. customto remove most of the methanol
  6. customto give a residue
  7. customto give a solid
  8. customDecant the solvent
  9. additionadd diethyl ether (200 mL)
  10. customcollect the solid
  11. filtrationby filtration
  12. customto give
  13. customafter drying

출처 및 근거

ORD 기록
ord-bc415e0df799461eae7f451bbb496434
출처 데이터셋
uspto-grants-1999_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05932571

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