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Isovaleric Acid → 2-(3-iodo-1-tosyl-1H-indol-5-yl)-5-isobutyl-1,3,4-oxadiazole

HRID 634218
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HRID 634218 반응식
[I:1][C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([C:11]([NH:13][NH2:14])=[O:12])[CH:9]=2)[N:4]([S:15]([C:18]2[CH:24]=[CH:23][C:21]([CH3:22])=[CH:20][CH:19]=2)(=[O:17])=[O:16])[CH:3]=1.[CH3:25][CH:26]([CH2:28][C:29](O)=O)[CH3:27].C(N(C(C)C)C(C)C)C.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.O=P(Cl)(Cl)Cl>C1COCC1>[I:1][C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([C:11]3[O:12][C:29]([CH2:28][CH:26]([CH3:27])[CH3:25])=[N:14][N:13]=3)[CH:9]=2)[N:4]([S:15]([C:18]2[CH:24]=[CH:23][C:21]([CH3:22])=[CH:20][CH:19]=2)(=[O:16])=[O:17])[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 10430Isovaleric AcidHCID 24813Phosphorus oxychlorideHCID 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 683285283-iodo-1-tosyl-1H-indole-5-carbohydrazide

생성물 1

HCID 68328230
2-(3-iodo-1-tosyl-1H-indol-5-yl)-5-isobutyl-1,3,4-oxadiazole
수율 35%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

In a 150 mL RBF was weighed 3-iodo-1-tosyl-1H-indole-5-carbohydrazide (1.16 g, 2.55 mmol) followed by THF (20 mL), isovalerianic acid (0.29 mL, 2.55 mmol) (TCI America) and N-ethyl-N-isopropylpropan-2-amine (1.11 mL, 6.37 mmol). To this stirring suspension was added HATU (1.07 g, 2.80 mmol) in one portion and the solution was stirred at RT for 2 h. The mixture was concentrated and treated with POCl3 (10 mL, 107 mmol) under argon. The flask was fitted with a reflux condenser and the reaction was heated to 110° C. for 14 h. The excess POCl3 was removed under reduced pressure and the crude residue was treated with EtOAc and a saturated solution of NaHCO3. It was extracted with EtOAc (50 mL) and washed with brine and dried over MgSO4, filtered and concentrated. The crude material was purified by flash chromatography (0-50% EtOAc in Hex) affording 2-(3-iodo-1-tosyl-1H-indol-5-yl)-5-isobutyl-1,3,4-oxadiazole (277 mg, 35%) as a white amorphous solid. MS (ESI, pos. ion) m/z: 522.0 (M+H)1. 1H NMR (400 MHz, DMSO-d6) δ ppm 8.24 (s, 1H), 8.17 (d, J=8.6 Hz, 1H), 8.03 (d, J=8.8 Hz, 1H), 7.97 (m, J=8.2 Hz, 2H), 7.87 (s, 1H), 7.43 (m, J=8.2 Hz, 2H), 2.84 (d, J=7.0 Hz, 2H), 2.33 (s, 3H), 2.15 (dt, J=13.5, 6.8 Hz, 1H), 0.99 (d, J=6.7 Hz, 6H).

후처리

  1. concentrationThe mixture was concentrated
  2. customThe flask was fitted with a reflux condenser
  3. temperaturethe reaction was heated to 110° C. for 14 h
  4. customThe excess POCl3 was removed under reduced pressure
  5. additionthe crude residue was treated with EtOAc
  6. extractionIt was extracted with EtOAc (50 mL)
  7. washwashed with brine
  8. dry with materialdried over MgSO4
  9. filtrationfiltered
  10. concentrationconcentrated
  11. customThe crude material was purified by flash chromatography (0-50% EtOAc in Hex)

출처 및 근거

ORD 기록
ord-03258034e8a54189baa0439283e26b8e
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09321756B2

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