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Hydrochloric Acid → HCID 178492478, 화합물

HRID 16759
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HRID 16759 반응식
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:15]=[C:16]([CH:20]=[CH:21][CH:22]=2)[C:17]([OH:19])=O)[CH2:10][CH2:9]1)=O)(C)(C)C.[NH2:23][C:24]1[N:28](C(OC(C)(C)C)=O)[N:27]=[C:26]([O:36][CH2:37][C:38]2[CH:43]=[C:42]([O:44][CH3:45])[CH:41]=[C:40]([O:46][CH3:47])[CH:39]=2)[CH:25]=1.N1C=CC=CC=1.Cl>C1COCC1.O1CCOCC1>[CH3:45][O:44][C:42]1[CH:43]=[C:38]([CH2:37][O:36][C:26]2[NH:27][N:28]=[C:24]([NH:23][C:17](=[O:19])[C:16]3[CH:20]=[CH:21][CH:22]=[C:14]([N:11]4[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]4)[CH:15]=3)[CH:25]=2)[CH:39]=[C:40]([O:46][CH3:47])[CH:41]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 448287263-(4-(Tert-butoxycarbonyl)piperazin-1-yl)benzoic acidHCID 66589741Tert-butyl 5-amino-3-[(3,5-dimethoxyphenyl)methoxy]pyrazole-1-carboxylate

생성물 1

HCID 178492478HCID 178492478, 화합물수율 12.6%

시약·촉매·용매 2

HCID 8028
Tetrahydrofuran
용매
HCID 312751,4-Dioxane용매

실험 절차

1-Chloro-N,N-2-trimethyl-1-propenylamine (78 μl, 0.588 mmol, 1.2 eq) was added dropwise to a stirred solution of 3-[4-(tert-butoxycarbonyl)piperazin-1-yl]benzoic acid (150 mg, 0.588 mmol, 1.2 eq) in THF (10 ml) under nitrogen. The mixture was stirred at room temperature overnight. tert-Butyl 5-amino-3-[(3,5-dimethoxyphenyl)methoxy]pyrazole-1-carboxylate (172 mg, 0.490 mmol, 1 eq) and pyridine (48 μl, 0.588 mol, 1.2 eq) were added and the mixture was heated at 65° C. overnight. The mixture was allowed to cool to room temperature and 4M HCl in dioxane (2 ml) was added. Stirring was continued at room temperature overnight. The precipitated yellow solid was collected by filtration and washed with THF. The solid was triturated with aq NaHCO3 (4 ml) and DCM (2 ml). A small amount of a brown gum remained out of solution. The gum was collected by filtration and washed with water and ether. The aqueous filtrate was extracted with ethyl acetate (3×10 ml) and the combined extracts were dried over MgSO4, filtered and evaporated. The extracted product was combined with the gum from filtration and purified by silica column chromatography, eluting with a gradient of 10-12% MeOH in DCM. Product fractions were evaporated to give the title compound as a white solid (27 mg, 10% yield); 1H NMR (399.902 MHz, DMSO+d4-AcOD) δ 3.13-3.21 (m, 4H), 3.33-3.40 (m, 4H), 3.68 (s, 6H), 5.02 (s, 2H), 5.71 (s, 1H), 6.38 (t, 1H), 6.52 (d, 2H), 7.12-7.17 (m, 1H), 7.33 (t, 1H), 7.37-7.41 (m, 1H), 7.46-7.49 (m, 1H). MS: m/z 438 (MH+)

후처리

  1. temperaturethe mixture was heated at 65° C. overnight
  2. temperatureto cool to room temperature
  3. stirringStirring
  4. waitwas continued at room temperature overnight
  5. filtrationThe precipitated yellow solid was collected by filtration
  6. washwashed with THF
  7. customThe solid was triturated with aq NaHCO3 (4 ml) and DCM (2 ml)
  8. filtrationThe gum was collected by filtration
  9. washwashed with water and ether
  10. extractionThe aqueous filtrate was extracted with ethyl acetate (3×10 ml)
  11. dry with materialthe combined extracts were dried over MgSO4
  12. filtrationfiltered
  13. customevaporated
  14. filtrationThe extracted product was combined with the gum from filtration
  15. custompurified by silica column chromatography
  16. washeluting with a gradient of 10-12% MeOH in DCM
  17. customProduct fractions were evaporated

출처 및 근거

ORD 기록
ord-6d123fcf353f4b5f92682a72c5b088e2
출처 데이터셋
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07737149B2

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