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Allyl bromide → 1-Allyl-2-(4-(tert-butoxycarbonyl)pyridin-3-yl)-3-cyclohexyl-1h-indole-6-carboxylic acid

HRID 860735
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HRID 860735 반응식
[H-].[Na+].[C:3]([O:7][C:8]([C:10]1[CH:15]=[CH:14][N:13]=[CH:12][C:11]=1[C:16]1[NH:17][C:18]2[C:23]([C:24]=1[CH:25]1[CH2:30][CH2:29][CH2:28][CH2:27][CH2:26]1)=[CH:22][CH:21]=[C:20]([C:31]([O:33]C)=[O:32])[CH:19]=2)=[O:9])([CH3:6])([CH3:5])[CH3:4].[CH2:35](Br)[CH:36]=[CH2:37]>CN(C=O)C.C1COCC1.CO.[OH-].[Na+]>[CH2:37]([N:17]1[C:18]2[C:23](=[CH:22][CH:21]=[C:20]([C:31]([OH:33])=[O:32])[CH:19]=2)[C:24]([CH:25]2[CH2:26][CH2:27][CH2:28][CH2:29][CH2:30]2)=[C:16]1[C:11]1[CH:12]=[N:13][CH:14]=[CH:15][C:10]=1[C:8]([O:7][C:3]([CH3:6])([CH3:4])[CH3:5])=[O:9])[CH:36]=[CH2:35]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 7841Allyl bromideHCID 24758Sodium hydrideHCID 69207220Methyl 2-(4-(tert-butoxycarbonyl)pyridin-3-yl)-3-cyclohexyl-1H-indole-6-carboxylate

생성물 1

HCID 692078291-Allyl-2-(4-(tert-butoxycarbonyl)pyridin-3-yl)-3-cyclohexyl-1h-indole-6-carboxylic acid

시약·촉매·용매 3

HCID 6228Dimethylformamide용매
HCID 14798
Sodium Hydroxide
용매
HCID 21899815MeOH tetrahydrofuran용매

실험 절차

To a suspension of NaH (19.5 mg of 60% dispersion in mineral oil, 0.488 mmol) in DMF (2 mL), methyl 2-(4-(tert-butoxycarbonyl)pyridin-3-yl)-3-cyclohexyl-1H-indole-6-carboxylate (100 mg, 0.222 mmol) was added and the reaction mixture was stirred at rt for 10 min. Allyl bromide (0.040 mL, 0.466 mmol) was then added, and the reaction mixture was stirred at rt for 3 hr. It was then quenched by the addition of water and acidified using 1N HCl solution. A yellowish precipitate formed which was collected by filtration to give the crude ester product in sufficient purity to proceed to the next step. This material was then dissolved in a THF/Methanol mixture (3 mL/3 mL) and 2N NaOH solution (2 mL) was added. The reaction mixture was heated at 100° C. under microwave conditions for 15 min. It was then concentrated and the pH was adjusted to 4–5 using 1N HCl solution. This mixture was then extracted using ethyl acetate and the organic layer was dried with MgSO4, filtered and evaporated and the resultant residue was purified using Prep. reverse phase HPLC to afford the title compound as a yellow solid, (50 mg, 44% yield two steps). MS m/z 516(MH+); 1H NMR (500 MHz, CD3OD) □ ppm 1.22–1.48 (m, 13 H) 1.70–2.02 (m, 5 H) 2.15 (m, 1 H) 2.37 (m, 1 H) 3.88 (dd, J=16.63, 5.04 Hz, 1 H) 4.13 (m, 1 H) 4.51 (m, 1 H) 4.76 (m, 1 H) 4.87 (m, 1 H) 5.04–5.21 (m, 3 H) 5.79 (m, 1 H) 5.97 (m, 1 H) 7.58 (d, J=5.80 Hz, 1 H) 7.78 (m, 1 H) 7.90 (d, J=8.24 Hz, 1 H) 8.13 (s, 1 H) 8.50 (s, 1 H) 8.67 (d, J=5.80 Hz, 1 H).

후처리

  1. additionwas added
  2. stirringthe reaction mixture was stirred at rt for 3 hr
  3. customIt was then quenched by the addition of water
  4. customA yellowish precipitate formed which
  5. filtrationwas collected by filtration
  6. customto give the crude ester product in sufficient purity
  7. additionwas added
  8. temperatureThe reaction mixture was heated at 100° C. under microwave conditions for 15 min
  9. concentrationIt was then concentrated
  10. extractionThis mixture was then extracted
  11. dry with materialthe organic layer was dried with MgSO4
  12. filtrationfiltered
  13. customevaporated
  14. customthe resultant residue was purified

출처 및 근거

ORD 기록
ord-677faba54a904dca9150ef33f59d4afa
출처 데이터셋
uspto-grants-2006_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07153848B2

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