Acetyl chloride → HCID 66745169、化合物

HRID 591653ノート

反応式

HRID 591653 の反応式
[CH:1]([NH:4][CH:5]1[CH2:10][CH2:9][N:8]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:7][CH2:6]1)([CH3:3])[CH3:2].CCN(CC)CC.[C:25](Cl)(=[O:27])[CH3:26]>C(Cl)Cl>[CH:1]([N:4]([CH:5]1[CH2:6][CH2:7][N:8]([C:11]([O:13][C:14]([CH3:15])([CH3:17])[CH3:16])=[O:12])[CH2:9][CH2:10]1)[C:25](=[O:27])[CH3:26])([CH3:3])[CH3:2]

参加物

5

反応物 3

HCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 20801236tert-Butyl 4-[(propan-2-yl)amino]piperidine-1-carboxylate

生成物 1

HCID 66745169HCID 66745169、化合物収率 59.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a 0° C. solution of tert-butyl 4-(isopropylamino)piperidine-1-carboxylate (1.2 g, 5.19 mmol) in CH2Cl2 (18 mL) was added Et3N (1.44 mL, 10.38 mmol) followed by acetyl chloride (0.55 mL, 7.78 mmol). The resulting solution was stirred for 2.5 hours, then concentrated in vacuo. The material was purified by flash chromatography on silica gel, eluting with 0% to 5% of EtOAc/CH2Cl2, to afford tert-butyl 4-(N-isopropylacetamido)piperidine-1-carboxylate (0.88 g, 59%).

後処理

  1. concentrationconcentrated in vacuo
  2. customThe material was purified by flash chromatography on silica gel
  3. washeluting with 0% to 5% of EtOAc/CH2Cl2

出典と根拠

ORDレコード
ord-060ac4bd04dc4d37ab025f0b7a3d2459
出典データセット
uspto-grants-2016_01
特許番号
US09238640B2

反応ノート

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