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Piperidine → 2-(2-Piperidin-1-ylmethyl-1H-indol-6-yloxy)-thiazolo[4,5-b]pyridine

HRID 1947523
ノート
印刷プレビュー

反応式

HRID 1947523 の反応式
[S:1]1[C:9]2[C:4](=[N:5][CH:6]=[CH:7][CH:8]=2)[N:3]=[C:2]1[O:10][C:11]1[CH:19]=[C:18]2[C:14]([CH:15]=[C:16]([CH:20]=O)[NH:17]2)=[CH:13][CH:12]=1.[NH:22]1[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]1.[BH-](OC(C)=O)(OC(C)=O)OC(C)=O.[Na+]>C(Cl)Cl>[N:22]1([CH2:20][C:16]2[NH:17][C:18]3[C:14]([CH:15]=2)=[CH:13][CH:12]=[C:11]([O:10][C:2]2[S:1][C:9]4[C:4]([N:3]=2)=[N:5][CH:6]=[CH:7][CH:8]=4)[CH:19]=3)[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8082PiperidineHCID 5049666Sodium triacetoxyborohydrideHCID 595776126-(Thiazolo[4,5-b]pyridin-2-yloxy)-1H-indole-2-carbaldehyde

生成物 1

HCID 498328182-(2-Piperidin-1-ylmethyl-1H-indol-6-yloxy)-thiazolo[4,5-b]pyridine収率 13%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a suspension of 6-(thiazolo[4,5-b]pyridin-2-yloxy)-1H-indole-2-carbaldehyde (76 mg, 0.26 mmol) in DCM (3 mL) was added piperidine (0.05 mL, 43 mg, 0.51 mmol), Na(OAc)3BH (65 mg, 0.31 mmol) and the reaction mixture was stirred (rt, 12 h). The reaction mixture was partitioned between saturated NaHCO3 (10 ml) and DCM (20 mL). The organic layer was separated and the aqueous layer was extracted with DCM (2×25 mL). The organic layer was dried, filtered and concentrated in vacuo. The resulting residue was purified by reverse phase HPLC to provide the title compound as a colorless solid (12 mg, 13%). MS (ESI): mass calcd. for C20H20N4OS, 364.1; m/z found, 365.1 [M+H]+. 1H NMR (500 MHz, CDCl3/CD3OD, 10/1): 8.51 (d, J=4.8, 1H), 7.97 (d, J=7.9, 1H), 7.54 (d, J=8.5, 1H), 7.40 (s, 1H), 7.18 (dd, J=7.9, 4.9, 1H), 7.02 (d, J=8.5, 1H), 6.36 (s, 1H), 3.63 (s, 2H), 2.53-2.47 (m, 2H), 2.47-2.36 (m, 2H), 1.76-1.44 (m, 6H).

後処理

  1. customThe reaction mixture was partitioned between saturated NaHCO3 (10 ml) and DCM (20 mL)
  2. customThe organic layer was separated
  3. extractionthe aqueous layer was extracted with DCM (2×25 mL)
  4. customThe organic layer was dried
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe resulting residue was purified by reverse phase HPLC

出典と根拠

ORDレコード
ord-51f9dc061c83410fa3ec6629f9e9c57d
出典データセット
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08399465B2

反応ノート

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