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Methanol → tert-butyl 4-[5-(6-methoxypyridin-3-yl)-4H-1,2,4-triazol-3-yl]piperidine-1-carboxylate

HRID 605014
ノート
印刷プレビュー

反応式

HRID 605014 の反応式
[NH:1]([C:3]([CH:5]1[CH2:10][CH2:9][N:8]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:7][CH2:6]1)=O)[NH2:2].CO[C:20]1[CH:21]=[C:22]([C:26]#[N:27])[CH:23]=[N:24][CH:25]=1.[CH3:28][O-:29].[Na+].CO>C(OCCO)C.C(O)(=O)C>[CH3:28][O:29][C:25]1[N:24]=[CH:23][C:22]([C:26]2[NH:27][C:3]([CH:5]3[CH2:10][CH2:9][N:8]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:7][CH2:6]3)=[N:1][N:2]=2)=[CH:21][CH:20]=1
参加物反応条件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 887MethanolHCID 10942334Sodium MethoxideHCID 22713165tert-Butyl 4-(hydrazinecarbonyl)piperidine-1-carboxylateHCID 231597785-Methoxypyridine-3-carbonitrile

生成物 1

HCID 178489121tert-butyl 4-[5-(6-methoxypyridin-3-yl)-4H-1,2,4-triazol-3-yl]piperidine-1-carboxylate

試薬・触媒・溶媒 2

HCID 176
Acetic Acid
溶媒
HCID 8076Glycol monoethyl ether溶媒

反応条件

温度
130 °C

実験手順

tert-Butyl 4-(hydrazinocarbonyl)-piperidine-1-carboxylate (800 mg, 3.29 mmol) was dissolved in anhydrous 2-ethoxyethanol (10 mL) and 5-methoxypyridine-3-carbonitrile (662 mg, 4.9 mmol) was added to the solution. A solution of 0.5M sodium methoxide in methanol (3 mL, ˜1.5 mmol) was added and the mixture was heated at 130° C. for 16 h. The cooled reaction mixture was neutralized with acetic acid and partitioned between ethyl acetate and aq. NaHCO3. The organic layer was dried over Na2SO4, the salts removed by filtration and the solvent evaporated under vacuum. This residue was triturated with diethyl ether to give tert-butyl 4-[5-(6-methoxypyridin-3-yl)-4H-1,2,4-triazol-3-yl]piperidine-1-carboxylate as a white solid. This material was dissolved in methylene chloride (10 mL) and TFA (10 mL) was added. After one hour the solvent was evaporated under reduced pressure to give 2-methoxy-5-(5-piperidin-4-yl-4H-1,2,4-triazol-3-yl)pyridine. NMR (MeOD): δ 8.75 (1H, s), 8.19 (1H, d, J=6 Hz), 6.93 (1H, d, J=6 Hz), 3.95 (3H, s), 3.51 (2H, m), 3.22 (3H, m), 2.32 (2H, m), 2.11 (2H, m).

後処理

  1. customThe cooled reaction mixture
  2. custompartitioned between ethyl acetate and aq. NaHCO3
  3. dry with materialThe organic layer was dried over Na2SO4
  4. customthe salts removed by filtration
  5. customthe solvent evaporated under vacuum
  6. customThis residue was triturated with diethyl ether

出典と根拠

ORDレコード
ord-07bdc3c61365467cab3a7c1749673ca9
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07910561B2

反応ノート

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