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1,2-Dichloroethane → HCID 178487650, 화합물

HRID 526463
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HRID 526463 반응식
C(C1[CH:8]=[CH:7][C:6]([C:9]2[CH:10]=[N:11][N:12]([C:15]3[CH:23]=[CH:22][C:18]([C:19]([OH:21])=O)=[CH:17][N:16]=3)[C:13]=2[OH:14])=[CH:5][CH:4]=1)#N.C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1.CC[N:40](C(C)C)C(C)C.[NH2:47][CH:48]1[CH2:53][CH2:52][N:51](C(OC(C)(C)C)=O)[CH2:50][CH2:49]1.[C:61]([OH:67])(C(F)(F)F)=O>CO.C(Cl)Cl.CC(N(C)C)=O>[OH:14][C:13]1[N:12]([C:15]2[CH:23]=[CH:22][C:18]([C:19]([NH:47][CH:48]3[CH2:49][CH2:50][NH:51][CH2:52][CH2:53]3)=[O:21])=[CH:17][N:16]=2)[N:11]=[CH:10][C:9]=1[C:6]1[CH:5]=[CH:4][N:40]=[C:8]([O:67][CH3:61])[CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 6

HCID 111,2-DichloroethaneHCID 6422Trifluoroacetic acidHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 12682914-Amino-1-Boc-piperidineHCID 178509615HCID 178509615, 화합물

생성물 1

HCID 178487650
HCID 178487650, 화합물
수율 62%

시약·촉매·용매 3

HCID 887Methanol용매HCID 6344Dichloromethane용매HCID 31374Dimethylacetamide용매

실험 절차

Combined 6-(4-(4-cyanophenyl)-5-hydroxy-1H-pyrazol-1-yl)nicotinic acid (50 mg, 0.163 mmol), EDC (46.9 mg, 0.245 mmol) and HOBT (37.5 mg, 0.245 mmol) and DMA (1 mL), and treated with Hunig's base (0.114 ml, 0.653 mmol) and stirred at ambient temperature for 5 minutes, then added to 4-amino-1-Boc-piperidine (38.5 mg, 0.327 mmol) and stirred at room temperature overnight. The reaction mixture was then diluted to a total volume of about 1.5 mL with methanol and purified via prep HPLC. The product containing fractions were collected and concentrated in vacuum to give a residue which was treated with TFA (2 mL) in DCM (2 mL). After stirring at ambient temperature overnight the reaction was concentrated in vacuo and dried under vacuum to give the title compound (39.3 mg, 62%) as a yellow solid. 1H NMR (400 MHz, DMSO-d6) δ ppm 1.65-1.82 (m, 2H) 1.93-2.08 (m, 2H) 2.94-3.16 (m, 2H) 3.35 (d, J=12.63 Hz, 2H) 3.99-4.19 (m, 1H) 7.80 (d, J=8.59 Hz, 2H) 8.15 (d, J=7.33 Hz, 2H) 8.29-8.78 (m, 6H) 8.87-8.99 (m, 1H) 13.59 (br. s., 1H). MS m/z [M+H]+ 389.2.

후처리

  1. stirringstirred at room temperature overnight
  2. custompurified via prep HPLC
  3. additionThe product containing fractions
  4. customwere collected
  5. concentrationconcentrated in vacuum
  6. customto give a residue which
  7. stirringAfter stirring at ambient temperature overnight the reaction
  8. concentrationwas concentrated in vacuo
  9. customdried under vacuum

출처 및 근거

ORD 기록
ord-86eb22b3685246f8aa4d12507a2f7b06
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09345713B2

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