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Tetrahydrofuran → 1-Tert-butyl 4-ethyl 4-(3-((methanesulfonyl)oxy)propyl)piperidine-1,4-dicarboxylate

HRID 39669
ノート
印刷プレビュー

反応式

HRID 39669 の反応式
O1CCCC1.[OH:6][CH2:7][CH2:8][CH2:9][C:10]1([C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH2:15][CH2:14][N:13]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:12][CH2:11]1.C(N(CC)CC)C.[CH3:35][S:36](Cl)(=[O:38])=[O:37]>O.C(OCC)(=O)C>[CH3:35][S:36]([O:6][CH2:7][CH2:8][CH2:9][C:10]1([C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH2:15][CH2:14][N:13]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:12][CH2:11]1)(=[O:38])=[O:37]
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 8028TetrahydrofuranHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 578152391-Tert-butyl 4-ethyl 4-(3-hydroxypropyl)piperidine-1,4-dicarboxylate

生成物 1

HCID 578155261-Tert-butyl 4-ethyl 4-(3-((methanesulfonyl)oxy)propyl)piperidine-1,4-dicarboxylate

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

To 20 mL of a tetrahydrofuran solution containing 1.7 g of 1-tert-butyl 4-ethyl 4-(3-hydroxypropyl)piperidine-1,4-dicarboxylate, 0.82 mL of triethylamine and 0.58 mL of methane sulfonylchloride were added at 5° C., and the mixture was stirred at room temperature for 1 hour. Ethyl acetate and water were added thereto. The organic layer was separated, and the aqueous layer was extracted with ethyl acetate. The organic layer and the extract were combined, the resultant solution was washed with an aqueous saturated sodium chloride solution and dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure to obtain 1.9 g of a colorless oily substance, 1-tert-butyl 4-ethyl 4-(3-((methanesulfonyl)oxy)propyl)piperidine-1,4-dicarboxylate.

後処理

  1. additionwere added at 5° C.
  2. customThe organic layer was separated
  3. extractionthe aqueous layer was extracted with ethyl acetate
  4. washthe resultant solution was washed with an aqueous saturated sodium chloride solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-93e876b0154a43d2a9ecd0e7b7dab8bb
出典データセット
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08524738B2

反応ノート

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