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Sodium hydride → (S)-methyl 1-(2-(quinuclidin-3-ylamino)ethyl)-1H-indazole-7-carboxylate

HRID 2369875
ノート
印刷プレビュー

反応式

HRID 2369875 の反応式
Cl.Cl.[NH2:3][C@H:4]1[CH:9]2[CH2:10][CH2:11][N:6]([CH2:7][CH2:8]2)[CH2:5]1.[H-].[Na+].C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].O=[CH:29][CH2:30][N:31]1[C:39]2[C:34](=[CH:35][CH:36]=[CH:37][C:38]=2[C:40]([O:42][CH3:43])=[O:41])[CH:33]=[N:32]1>C1COCC1.C(O)(=O)C>[N:6]12[CH2:11][CH2:10][CH:9]([CH2:8][CH2:7]1)[C@H:4]([NH:3][CH2:29][CH2:30][N:31]1[C:39]3[C:34](=[CH:35][CH:36]=[CH:37][C:38]=3[C:40]([O:42][CH3:43])=[O:41])[CH:33]=[N:32]1)[CH2:5]2
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 4

HCID 24758Sodium hydrideHCID 5049666Sodium triacetoxyborohydrideHCID 12494973(3S)-1-azabicyclo[2.2.2]octan-3-amine dihydrochlorideHCID 86672700methyl 1-(2-oxoethyl)-1H-indazole-7-carboxylate

生成物 1

HCID 66899049(S)-methyl 1-(2-(quinuclidin-3-ylamino)ethyl)-1H-indazole-7-carboxylate

試薬・触媒・溶媒 2

HCID 176
Acetic Acid
溶媒
HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a stirred solution of (S)-(−)-3-aminoquinuclidine dihydrochloride (0.3 g, 1.3 mmol) in THF (13 mL) was added sodium hydride (0.1 g, 2.7 mmol) and the mixture was stirred for 1.5 h. Acetic acid (0.5 mL) and sodium triacetoxyborohydride (380 mg, 1.8 mmol) were added and stirred for 0.5 h. A solution of methyl 1-(2-oxoethyl)-1H-indazole-7-carboxylate (0.3 g, 1.3 mmol) from Step E above in THF (13 mL) was added dropwise, and the resulting suspension was stirred overnight at ambient temperature. The solvent was removed under reduced pressure, and the crude material was purified by preparative thin layer chromatography (90:9:1 methylene chloride/methanol/concentrated ammonium hydroxide) to afford (S)-methyl 1-(2-(quinuclidin-3-ylamino)ethyl)-1H-indazole-7-carboxylate: 1H NMR (500 MHz, DMSO-d6) δ 8.25 (s, 1H), 8.03 (dd, J=8.0, 1.0 Hz, 1H), 7.85 (dd, J=7.0, 1.0 Hz, 1H), 7.22 (t, J=7.5 Hz, 1H), 4.68-4.65 (m, 2H), 3.94 (s, 3H), 2.84-2.70 (m, 3H), 2.64-2.45 (m, 2H), 2.03-1.99 (m, 2H), 1.86-1.75 (m, 2H), 1.58-1.51 (m, 3H), 1.45-1.32 (m, 1H), 1.08-1.01 (m, 1H); MS (ESI+) m/z 329 (M+H).

後処理

  1. stirringstirred for 0.5 h
  2. stirringthe resulting suspension was stirred overnight at ambient temperature
  3. customThe solvent was removed under reduced pressure
  4. customthe crude material was purified by preparative thin layer chromatography (90:9:1 methylene chloride/methanol/concentrated ammonium hydroxide)

出典と根拠

ORDレコード
ord-53a1afb1f4a04468ab8d8bf597b2bc12
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08710046B2

反応ノート

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