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Cyclopentylamine → HCID 44234766、化合物

HRID 1093791
ノート
印刷プレビュー

反応式

HRID 1093791 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 6

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

生成物 1

HCID 44234766
HCID 44234766、化合物
収率 55%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-4fc2633cb1e048f592698b6960128ec6
出典データセット
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08129376B2

反応ノート

読み込み中…

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