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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Triethylamine → (3-(4-(6-Oxa-2-azaspiro[3.4]octan-2-ylmethyl)-3-methylphenoxy)azetidin-1-yl)(5-phenyl-1,3,4-oxadiazol-2-yl)methanone

HRID 2359373
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HRID 2359373 반응식
Cl.[CH2:2]1[C:5]2([CH2:9][CH2:8][O:7][CH2:6]2)[CH2:4][NH:3]1.C(N(CC)CC)C.[CH3:17][C:18]1[CH:25]=[C:24]([O:26][CH:27]2[CH2:30][N:29]([C:31]([C:33]3[O:34][C:35]([C:38]4[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=4)=[N:36][N:37]=3)=[O:32])[CH2:28]2)[CH:23]=[CH:22][C:19]=1[CH:20]=O.[Na].C([O-])(O)=O.[Na+]>ClCCl>[CH2:2]1[C:5]2([CH2:9][CH2:8][O:7][CH2:6]2)[CH2:4][N:3]1[CH2:20][C:19]1[CH:22]=[CH:23][C:24]([O:26][CH:27]2[CH2:30][N:29]([C:31]([C:33]3[O:34][C:35]([C:38]4[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=4)=[N:36][N:37]=3)=[O:32])[CH2:28]2)=[CH:25][C:18]=1[CH3:17]
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참가 물질

7

반응물 5

HCID 8471TriethylamineHCID 516892Sodium BicarbonateHCID 5360545SodiumHCID 580431052-Methyl-4-(1-(5-phenyl-1,3,4-oxadiazole-2-carbonyl)azetidin-3-yloxy)benzaldehydeHCID 717440076-Oxa-2-azaspiro(3.4)octane hydrochloride

생성물 1

HCID 71226268
(3-(4-(6-Oxa-2-azaspiro[3.4]octan-2-ylmethyl)-3-methylphenoxy)azetidin-1-yl)(5-phenyl-1,3,4-oxadiazol-2-yl)methanone
수율 40%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

6-Oxa-2-azaspiro[3.4]octane HCl salt (0.064 g, 0.43 mmol) was dissolved in dichloromethane (2 ml). Triethylamine (0.064 ml, 0.47 mmol) was added, followed by 2-methyl-4-(1-(5-phenyl-1,3,4-oxadiazole-2-carbonyl)azetidin-3-yloxy)benzaldehyde (0.13 g, 0.36 mmol) and sodium triacetoxyhydroborate (0.152 g, 0.72 mmol). The mixture was stirred at ambient temperature overnight. The reaction mixture was diluted with dichloromethane (10 ml) and then shaken with NaHCO3. The two phases were separated by the use of a phase separator. Evaporation of dichloromethane afforded crude material, which was purified by preparative reverse-phase HPLC at pH 10 to give 66 mg (40%) of the desired product as a solid. 1H NMR (600 MHz, DMSO) δ 2.01 (t, 2H), 2.27 (s, 3H), 3.13 (q, 4H), 3.47 (s, 2H), 3.64 (t, 2H), 3.70 (d, 2H), 4.08 (dd, 1H), 4.51-4.56 (m, 1H), 4.63 (dd, 1H), 5.06-5.15 (m, 2H), 6.65 (dd, 1H), 6.71 (d, 1H), 7.18 (d, 1H), 7.62-7.73 (m, 3H), 8.06-8.11 (m, 2H). MS (APCI+) m/z 461.2 [M+H]+, LC purity: 98%

후처리

  1. customThe two phases were separated by the use of a phase separator
  2. customEvaporation of dichloromethane
  3. customafforded crude material, which
  4. customwas purified by preparative reverse-phase HPLC at pH 10

출처 및 근거

ORD 기록
ord-1f5f8176d14b49db927c8d26c4f97e30
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08685958B2

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