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Cyclopentylamine → HCID 44234766, 화합물

HRID 1093791
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HRID 1093791 반응식
CCN(C(C)C)C(C)C.[CH:10]1([N:15]2[CH:19]=[C:18]([C:20]([OH:22])=O)[N:17]=[N:16]2)[CH2:14][CH2:13][CH2:12][CH2:11]1.C1(N)CCCC1.C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.Cl.[NH2:51][CH2:52][C:53]([N:55]1[CH2:60][CH2:59][CH:58]([O:61][C:62]2[CH:63]=[N:64][CH:65]=[C:66]([Cl:68])[CH:67]=2)[CH2:57][CH2:56]1)=[O:54]>CN(C=O)C.O>[Cl:68][C:66]1[CH:67]=[C:62]([O:61][CH:58]2[CH2:57][CH2:56][N:55]([C:53](=[O:54])[CH2:52][NH:51][C:20]([C:18]3[N:17]=[N:16][N:15]([CH:10]4[CH2:11][CH2:12][CH2:13][CH2:14]4)[CH:19]=3)=[O:22])[CH2:60][CH2:59]2)[CH:63]=[N:64][CH:65]=1
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참가 물질

9

반응물 6

HCID 2906CyclopentylamineHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 62061226HCID 62061226, 화합물HCID 665916722-Amino-1-[4-(5-chloro-pyridin-3-yloxy)-piperidin-1-yl]-ethanone hydrochloride

생성물 1

HCID 44234766
HCID 44234766, 화합물
수율 55%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

DIPEA (300 mg, 2.3 mmol) was added to a stirred solution of 1-Cyclopentyl-1H-[1,2,3]triazole-4-carboxylic acid (75 mg, 0.41 mmol (prepared by the method used for the synthesis of Intermediate 64, starting from cyclopentylamine) in DMF (5 mL) followed by HOBt (61 mg, 0.4 mmol) and EDCI (200 mg, 1 mmol). After 2 minutes of stirring, 2-amino-1-[4-(5-chloro-pyridin-3-yloxy)-piperidin-1-yl]-ethanone hydrochloride (prepared according to Step 1 and 5 of the General Scheme) (156 mg, 0.5 mmol) was added and the resulting mixture was stirred at ambient temperature overnight. Cold water was then added and filtered the precipitate was filtered. The solid obtained was purified by recrystallisation from a solvent system EtOAc:hexane:MeOH (3:7:0.2) to afford 98 mg (55% Yield) of 1-cyclopentyl-1H-[1,2,3]triazole-4-carboxylic acid {2-[4-(5-chloro-pyridin-3-yloxy)-piperidin-1-yl]-2-oxo-ethyl}-amide. LC/MS [M+H]+ 433, 98.59%. 1H NMR (300 MHz, DMSO-d6): δ 8.7 (s, 1H), 8.34 (m, 2H), 8.24 (s, 1H), 7.74 (s, 1H), 5.1 (m, 1H), 4.9 (m, 1H), 4.2 (d, 2H), 4.0 (bs, 1H), 3.8 (bs, 1H), 3.4 (s, 1H), 3.3 (m, 1H), 2.3 (m, 2H), 2.1 (m, 4H), 1.9-1.5 (m, 6H).

후처리

  1. customprepared by the method
  2. additionwas added
  3. stirringthe resulting mixture was stirred at ambient temperature overnight
  4. filtrationfiltered the precipitate
  5. filtrationwas filtered
  6. customThe solid obtained
  7. customwas purified by recrystallisation from a solvent system EtOAc:hexane:MeOH (3:7:0.2)

출처 및 근거

ORD 기록
ord-4fc2633cb1e048f592698b6960128ec6
출처 데이터셋
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08129376B2

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