Methylamine → HCID 90136020、化合物

HRID 2275799ノート

反応式

HRID 2275799 の反応式
O=C1C2C(=CC=CC=2)C(=O)[N:3]1[CH:12]([CH2:25][O:26][CH:27]([CH3:29])[CH3:28])[CH2:13][NH:14][C:15](=[O:24])[O:16][CH2:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.CN>C(O)C>[NH2:3][CH:12]([CH2:25][O:26][CH:27]([CH3:29])[CH3:28])[CH2:13][NH:14][C:15](=[O:24])[O:16][CH2:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

参加物

4

反応物 2

HCID 6329MethylamineHCID 90136015HCID 90136015、化合物

生成物 1

HCID 90136020HCID 90136020、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
60 °C

実験手順

2.3 g of rac-benzyl [2-(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)-3-isopropoxypropyl]carbamate (5.6 mmol, 1 equivalent) were dissolved in 30 ml of ethanol, 7.3 ml of 40% strength aqueous methylamine solution (84.4 mmol, 15 equivalent) were added and the mixture was stirred at 60° C. overnight. The reaction mixture was concentrated and the residue was then chromatographed on silica gel (Biotage Isolera; mobile phase: dichloromethane/methanol gradient). This gave 730 mg (49% of theory) of the title compound.

後処理

  1. concentrationThe reaction mixture was concentrated
  2. customthe residue was then chromatographed on silica gel (Biotage Isolera; mobile phase: dichloromethane/methanol gradient)

出典と根拠

ORDレコード
ord-6ff07479a06141db929e6d6bde54de3d
出典データセット
uspto-grants-2015_09
特許番号
US09126998B2

反応ノート

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