1-Methyl-4-(methylamino)piperidine → HCID 68773722、化合物

HRID 1174530ノート

反応式

HRID 1174530 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:10]=1[NH:9][CH:8]=[C:7]2[C:11]([OH:13])=O.[CH3:14][N:15]1[CH2:20][CH2:19][CH:18]([NH:21][CH3:22])[CH2:17][CH2:16]1>ClCCl>[CH3:22][N:21]([CH:18]1[CH2:19][CH2:20][N:15]([CH3:14])[CH2:16][CH2:17]1)[C:11]([C:7]1[C:6]2[C:10](=[C:2]([Br:1])[CH:3]=[CH:4][CH:5]=2)[NH:9][CH:8]=1)=[O:13]

参加物

4

反応物 2

HCID 5663231-Methyl-4-(methylamino)piperidineHCID 248204637-Bromo-1H-indole-3-carboxylic acid

生成物 1

HCID 68773722HCID 68773722、化合物収率 31%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 7-Bromo-1H-indole-3-carboxylic acid (A) (240 mg, 1 mmol) in dichloromethane (8 cm3) was added polystyrene-bound carbodiimide (1 g, loading 1.3 mmol/g, 1.3 mmol) followed by 1-methyl-4-(methylamino)piperidine (192 mg, 1.5 mmol) and the resulting suspension was gently shaken at room temperature for 16 h. The suspension was filtered and the resin washed with dichloromethane. The filtrate was then washed with saturated aqueous sodium bicarbonate solution, water before the organic portion was dried over magnesium sulfate, filtered and the filtrate evaporated under reduced pressure to give the title compound (B) (107.2 mg, 31%).

後処理

  1. filtrationThe suspension was filtered
  2. washthe resin washed with dichloromethane
  3. washThe filtrate was then washed with saturated aqueous sodium bicarbonate solution, water before the organic portion
  4. dry with materialwas dried over magnesium sulfate
  5. filtrationfiltered
  6. customthe filtrate evaporated under reduced pressure

出典と根拠

ORDレコード
ord-be51d278a8604309ae528b77a2598c14
出典データセット
uspto-grants-2010_11
特許番号
US07838518B2

反応ノート

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