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Acetic Acid → tert-Butyl 7-[(5-methoxypyridin-2-yl)acetyl]-2,7-diazaspiro[3.5]nonane-2-carboxylate

HRID 1913448
ノート
印刷プレビュー

反応式

HRID 1913448 の反応式
Cl.[CH2:2]1[C:5]2([CH2:10][CH2:9][NH:8][CH2:7][CH2:6]2)[CH2:4][N:3]1[C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12].C([N:20]([CH2:23][CH3:24])[CH2:21][CH3:22])C.[C:25]([OH:28])(=O)[CH3:26].CN([C:32]([O:36]N1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.Cl[CH2:54]Cl>>[CH3:32][O:36][C:22]1[CH:54]=[CH:24][C:23]([CH2:26][C:25]([N:8]2[CH2:7][CH2:6][C:5]3([CH2:4][N:3]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:2]3)[CH2:10][CH2:9]2)=[O:28])=[N:20][CH:21]=1
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 5

HCID 176Acetic AcidHCID 6344DichloromethaneHCID 8471TriethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 24820549tert-Butyl 2,7-diazaspiro[3.5]nonane-2-carboxylate hydrochloride

生成物 1

HCID 58438449
tert-Butyl 7-[(5-methoxypyridin-2-yl)acetyl]-2,7-diazaspiro[3.5]nonane-2-carboxylate
収率 96%

実験手順

In an oven dried round-bottomed flask was suspended tert-butyl 2,7-diazaspiro[3.5]nonane-2-carboxylate hydrochloride (1.89 g, 7.18 mmol) in anhydrous dichloromethane (50 mL). Triethylamine (2 mL, 14.4 mmol) followed by 5-methoxypyridin-2-yl)acetic acid (SM-1aa, 1.2 g, 7.18 mmol) were added. HATU (3.28 g, 8.62 mmol) was added and the resulting bright yellow solution was stirred at room temperature for 15 hours. The reaction mixture was washed consecutively with saturated aqueous sodium bicarbonate, water and brine and was dried over anhydrous MgSO4. Filtration and solvent removal afforded the crude material as a brownish oil (4.8 g). The product was purified by silica chromatography using a Combiflash ISCO (Teledyne Isco Inc., Lincoln, Nebr.) system to give the title compound (2-1a) as a light yellow foam (2.57 g, 96%). MS (ES+) 376.4 (M+H)+. 1H NMR (CDCl3) δ 1.42 (s, 9H), 1.57-1.61 (m, 2H), 1.65-1.69 (m, 2H), 3.47-3.54 (m, 4H), 3.58-3.64 (m, 4H), 3.83 (s, 3H), 3.85 (s, 2H), 7.15-7.18 (m, 1H), 7.23-7.26 (m, 1H), 8.18 (d, 1H).

後処理

  1. customIn an oven dried round-bottomed flask was suspended
  2. additionwere added
  3. washThe reaction mixture was washed consecutively with saturated aqueous sodium bicarbonate, water and brine
  4. dry with materialwas dried over anhydrous MgSO4
  5. filtrationFiltration and solvent removal
  6. customafforded the crude material as a brownish oil (4.8 g)
  7. customThe product was purified by silica chromatography

出典と根拠

ORDレコード
ord-af08487eb50c404f843080a2cfb984a0
出典データセット
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08609680B2

反応ノート

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