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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
ノート
印刷プレビュー

反応式

HRID 2359373 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 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

生成物 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
収率 40%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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%

後処理

  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

出典と根拠

ORDレコード
ord-1f5f8176d14b49db927c8d26c4f97e30
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08685958B2

反応ノート

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