1-Methyl-4-(methylamino)piperidine → HCID 68773722, 화합물

HRID 1174530노트

반응식

HRID 1174530 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 68773722HCID 68773722, 화합물수율 31%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-be51d278a8604309ae528b77a2598c14
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07838518B2

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