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Acetic Acid → HCID 178453912、化合物

HRID 2042404
ノート
印刷プレビュー

反応式

HRID 2042404 の反応式
[C:1]([O:5][C:6](=[O:17])[NH:7][C@H:8]1[CH2:13][CH2:12][C@H:11]([CH2:14][CH:15]=O)[CH2:10][CH2:9]1)([CH3:4])([CH3:3])[CH3:2].[N:18]1([C:24]2[C:29]3[CH:30]=[CH:31][S:32][C:28]=3[CH:27]=[CH:26][N:25]=2)[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]1.CC(O)=O.C([O-])(O)=O.[Na+]>ClCCCl>[C:1]([O:5][C:6](=[O:17])[NH:7][C@H:8]1[CH2:13][CH2:12][C@H:11]([CH2:14][CH2:15][N:21]2[CH2:22][CH2:23][N:18]([C:24]3[C:29]4[CH:30]=[CH:31][S:32][C:28]=4[CH:27]=[CH:26][N:25]=3)[CH2:19][CH2:20]2)[CH2:10][CH2:9]1)([CH3:4])([CH3:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 176Acetic AcidHCID 516892Sodium BicarbonateHCID 109660274-(Piperazin-1-yl)thieno[3,2-c]pyridineHCID 178453924HCID 178453924、化合物

生成物 1

HCID 178453912HCID 178453912、化合物収率 72%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane
溶媒

実験手順

trans-[4-(2-oxo-ethyl)-cyclohexyl]-carbamic acid tert-butyl ester [CAS-Nr. 215790-29-7] (1.0 g, 4 mmol) was added to a solution under N2 of commercially available 4-piperazine-1-yl-thieno[3,2-c]pyridine [CAS-Nr. 106261-27-2] (0.85 g, 4 mmol) in 1,2-dichloroethane (45 ml) and AcOH (0.22 ml, 4 mmol). The resulting reaction mixture was stirred 8 h at room temperature before addition of Na(AcO)3BH (1.2 g, 6 mmol). Stirring was continued over night at room temperature. Sat. aq. NaHCO3 sol. was added and the product was extracted with EtOAc (2×). The combined organic layers were washed with H2O and brine. After drying (MgSO4) the solvent was evaporated and the product was purified by flash chromatography on silica gel (CH2Cl2/MeOH, 100:0 to 90:10) to yield trans-{4-[2-(4-thieno[3,2-c]pyridin-4-yl-piperazin-1-yl)-ethyl]-cyclohexyl}-carbamic acid tert-butyl ester as a light yellow solid (1.2 g, 72%), MS (ISP) m/z=445.3 [(M+H)+].

後処理

  1. customThe resulting reaction mixture
  2. waitwas continued over night at room temperature
  3. extractionthe product was extracted with EtOAc (2×)
  4. washThe combined organic layers were washed with H2O and brine
  5. dry with materialAfter drying (MgSO4) the solvent
  6. customwas evaporated
  7. customthe product was purified by flash chromatography on silica gel (CH2Cl2/MeOH, 100:0 to 90:10)

出典と根拠

ORDレコード
ord-376ab6342ae54c34a29a6ea0289ab0a1
出典データセット
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08586579B2

反応ノート

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