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Potassium Sodium Tartrate → N-methoxy-N-methyl-2-[5-(methylsulfanyl)pyridin-2-yl]-3-(tetrahydro-2H-pyran-4-yl)propanamide

HRID 1881917
ノート
印刷プレビュー

反応式

HRID 1881917 の反応式
Cl.[CH3:2][O:3][NH:4][CH3:5].C[Al](C)C.[CH3:10][S:11][C:12]1[CH:13]=[CH:14][C:15]([CH:18]([CH2:24][CH:25]2[CH2:30][CH2:29][O:28][CH2:27][CH2:26]2)[C:19]([O:21]CC)=O)=[N:16][CH:17]=1.C(=O)([O-])O.[Na+].[C@H](O)(C([O-])=O)[C@@H](O)C([O-])=O.[Na+].[K+]>C1(C)C=CC=CC=1>[CH3:2][O:3][N:4]([CH3:5])[C:19](=[O:21])[CH:18]([C:15]1[CH:14]=[CH:13][C:12]([S:11][CH3:10])=[CH:17][N:16]=1)[CH2:24][CH:25]1[CH2:26][CH2:27][O:28][CH2:29][CH2:30]1
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 5

HCID 9357Potassium Sodium TartrateHCID 81138Methanamine, N-methoxy-, hydrochloride (1:1)HCID 516892Sodium BicarbonateHCID 16682925TrimethylaluminumHCID 59331616ethyl 2-[5-(methylsulfanyl)pyridin-2-yl]-3-(tetrahydro-2H-pyran-4-yl)propanoate

生成物 1

HCID 86641954
N-methoxy-N-methyl-2-[5-(methylsulfanyl)pyridin-2-yl]-3-(tetrahydro-2H-pyran-4-yl)propanamide
収率 25%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

A solution of N-methoxymethanamine hydrochloride (1.48 g) in toluene (15 mL) was cooled to 0° C., and trimethylaluminum (1.4M hexane solution, 10.9 mL) was added dropwise. The reaction mixture was stirred at room temperature for 1.5 hr, and a solution of ethyl 2-[5-(methylsulfanyl)pyridin-2-yl]-3-(tetrahydro-2H-pyran-4-yl)propanoate (1.57 g) in toluene (15 mL) was added dropwise. The reaction mixture was stirred at room temperature for 6 hr, saturated aqueous sodium hydrogen carbonate and saturated aqueous Rochelle salt solution were added and the mixture was stirred for 1 hr. The reaction mixture was extracted with ethyl acetate, and the ethyl acetate layer was washed with saturated brine, dried (MgSO4) and concentrated. The residue was subjected to silica gel column chromatography, and the title compound (404 mg, yield 25%) was obtained as a pale-yellow amorphous solid from a fraction eluted with ethyl acetate-hexane (9:1, volume ratio).

後処理

  1. stirringThe reaction mixture was stirred at room temperature for 6 hr
  2. stirringthe mixture was stirred for 1 hr
  3. extractionThe reaction mixture was extracted with ethyl acetate
  4. washthe ethyl acetate layer was washed with saturated brine
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-0012d9126f61405886582d4329e2120b
出典データセット
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08318746B2

反応ノート

読み込み中…

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