Water → HCID 66987744、化合物

HRID 333421

反応式

HRID 333421 の反応式
[CH:1]1([NH:4][CH:5]2[CH2:10][CH2:9][N:8]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:7][CH2:6]2)[CH2:3][CH2:2]1.C(N(CC)CC)C.[C:25](Cl)(=O)[CH2:26][CH3:27].[OH2:30]>C1COCC1>[CH:26]1([CH2:2][CH2:3][C:1]([NH:4][CH:5]2[CH2:6][CH2:7][N:8]([C:11]([O:13][C:14]([CH3:15])([CH3:16])[CH3:17])=[O:12])[CH2:9][CH2:10]2)=[O:30])[CH2:27][CH2:25]1

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 62324Propionyl chlorideHCID 2769591tert-Butyl 4-(cyclopropylamino)piperidine-1-carboxylate

生成物 1

HCID 66987744HCID 66987744、化合物収率 89%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

0.8 g (3.3 mmol) of tert-butyl 4-cyclopropylaminopiperidine-1-carboxylate, 0.48 mL (3.3 mmol) of triethylamine and 0.56 mL (3.3 mmol) of propionyl chloride are dissolved in 50 mL of THF. The reaction medium is stirred for 2 hours at room temperature. The reaction is stopped by adding water and the organic products are then extracted with dichloromethane. The organic phase is dried and then evaporated. The crude product obtained is chromatographed on silica gel (eluent: 6/4 heptane/ethyl acetate). 0.87 g of tert-butyl 4-(cyclopropylpropionylamino)piperidine-1-carboxylate in the form of a colourless oil is obtained in a yield of 89%.

後処理

  1. extractionthe organic products are then extracted with dichloromethane
  2. customThe organic phase is dried
  3. customevaporated
  4. customThe crude product obtained
  5. customis chromatographed on silica gel (eluent: 6/4 heptane/ethyl acetate)

出典と根拠

ORDレコード
ord-1de102abcc1d483ab3fa12abd58096c9
出典データセット
uspto-grants-2014_11
特許番号
US08877968B2

関連ノート

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