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Triethylamine → HCID 46178915, 화합물

HRID 1890724
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HRID 1890724 반응식
[O:1]=[C:2]1[NH:10][C:5]2=[N:6][CH:7]=[CH:8][CH:9]=[C:4]2[C@:3]21[CH2:42][C:13]1[CH:14]=[C:15]3[C:20](=[CH:21][C:12]=1[CH2:11]2)[N:19]=[CH:18][C:17]([CH2:22][NH:23][CH2:24][CH:25]([C:36]1[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1)[CH2:26][NH:27][C:28]1([C:33]([OH:35])=O)[CH2:32][CH2:31][CH2:30][CH2:29]1)=[CH:16]3.C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.C(N(CC)CC)C>C1COCC1>[O:35]=[C:33]1[C:28]2([CH2:32][CH2:31][CH2:30][CH2:29]2)[NH:27][CH2:26][CH:25]([C:36]2[CH:37]=[CH:38][CH:39]=[CH:40][CH:41]=2)[CH2:24][N:23]1[CH2:22][C:17]1[CH:18]=[N:19][C:20]2[C:15]([CH:16]=1)=[CH:14][C:13]1[CH2:42][C@:3]3([CH2:11][C:12]=1[CH:21]=2)[C:4]1[C:5](=[N:6][CH:7]=[CH:8][CH:9]=1)[NH:10][C:2]3=[O:1]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 58550626HCID 58550626, 화합물

생성물 1

HCID 46178915HCID 46178915, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 1-{[3-({[(7,5)-2′-oxo-1′,2′,6,8-tetrahydrospiro[cyclopenta[g]quinoline-7,3′-pyrrolo[2,3-b]pyridin]-3-yl]methyl}amino)-2-phenylpropyl]-amino}cyclopentanecarboxylic acid from Step F (30 mg, 0.053 mmol) and HOBt (8.2 mg, 0.053 mmol) in THF (1 mL) were added EDCI (13.3 mg, 0.069 mmol) and triethylamine (19 μL, 0.14 mmol). This solution was stirred at ambient temperature for 18 h. The solution was then concentrated to yield a residue, which was applied to a silica gel column for purification, eluting with a gradient of 1-7% methanol in DCM. Concentration of the fractions containing the product provided the title compound. MS: m/z=544 (M+1). HRMS: m/z=544.2708, calculated m/z=544.2707 for C34H34N5O2.

후처리

  1. concentrationThe solution was then concentrated
  2. customto yield a residue, which
  3. customwas applied to a silica gel column for purification
  4. washeluting with a gradient of 1-7% methanol in DCM
  5. additionConcentration of the fractions containing the product

출처 및 근거

ORD 기록
ord-dc2b30b4a433428a92edd5fdeef68b74
출처 데이터셋
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08507477B2

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