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tert-Butyl 4-oxopiperidine-1-carboxylate → 3-[2-(1-t-Butoxycarbonyl-4-piperidinylamino)ethyl]-2-aminopyridine

HRID 1453958
ノート
印刷プレビュー

反応式

HRID 1453958 の反応式
[NH2:1][CH2:2][CH2:3][C:4]1[C:5]([NH2:10])=[N:6][CH:7]=[CH:8][CH:9]=1.[C:11]([O:15][C:16]([N:18]1[CH2:23][CH2:22][C:21](=O)[CH2:20][CH2:19]1)=[O:17])([CH3:14])([CH3:13])[CH3:12].C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>ClC(Cl)C.C(O)(=O)C>[C:11]([O:15][C:16]([N:18]1[CH2:23][CH2:22][CH:21]([NH:1][CH2:2][CH2:3][C:4]2[C:5]([NH2:10])=[N:6][CH:7]=[CH:8][CH:9]=2)[CH2:20][CH2:19]1)=[O:17])([CH3:14])([CH3:12])[CH3:13]
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 3

HCID 735900tert-Butyl 4-oxopiperidine-1-carboxylateHCID 5049666Sodium triacetoxyborohydrideHCID 541059293-(2-Aminoethyl)pyridin-2-amine

生成物 1

HCID 685357713-[2-(1-t-Butoxycarbonyl-4-piperidinylamino)ethyl]-2-aminopyridine収率 42.2%

試薬・触媒・溶媒 2

HCID 176Acetic Acid触媒
HCID 6365
1,1-Dichloroethane
溶媒

実験手順

A solution of 3-(2-aminoethyl)-2-aminopyridine (0.122 g, 0.88 mmol) and 1-t-butoxycarbonyl 4-piperidone (0.177 g, 0.88 mmol) in dichloroethane (3 mL) containing 2 drops of acetic acid was treated with sodium triacetoxyborohydride (0.28 g, 1.33 mmol) at 20-75° C. until starting material was no longer consumed. The reaction was worked up with saturated sodium bicarbonate and methylene chloride, and dried over sodium sulfate. The crude product was purified by chromatography (silica gel, 0-10% {0.1% ammonium hydroxide in methanol) in methylene chloride, gradient elution) to produce the title compound (0.119 g) as a yellow oil. MS 321 (M+1).

後処理

  1. customwas no longer consumed
  2. dry with materialdried over sodium sulfate
  3. customThe crude product was purified by chromatography (silica gel, 0-10% {0.1% ammonium hydroxide in methanol) in methylene chloride
  4. washgradient elution)

出典と根拠

ORDレコード
ord-e64ae6b86b49456fb572f5d2fcbe7ae8
出典データセット
uspto-grants-2009_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07476665B2

反応ノート

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