Dimethylamine, hydrochloride → HCID 66805417, 화합물

HRID 1193354노트

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HRID 1193354 반응식
CS([C:5]1[N:6]=[CH:7][C:8]2[CH2:14][N:13]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:12][CH2:11][C:9]=2[N:10]=1)(=O)=O.Cl.[CH3:23][NH:24][CH3:25].CCN(C(C)C)C(C)C>CN1C(=O)CCC1.O>[CH3:23][N:24]([CH3:25])[C:5]1[N:6]=[CH:7][C:8]2[CH2:14][N:13]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:12][CH2:11][C:9]=2[N:10]=1

참가 물질

6

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HCID 10473Dimethylamine, hydrochlorideHCID 81531DiisopropylethylamineHCID 22709841tert-Butyl 7,8-dihydro-2-(methylsulfonyl)pyrido[4,3-d]pyrimidine-6(5H)-carboxylate

생성물 1

HCID 66805417HCID 66805417, 화합물수율 78%

시약·촉매·용매 2

HCID 962Water용매HCID 13387N-methyl-2-pyrrolidone용매

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온도
130 °C

실험 절차

A mixture of tert-butyl 2-(methylsulfonyl)-7,8-dihydropyrido[4,3-d]pyrimidine-6(5H)-carboxylate (2.8 g, 8.95 mmol, 1.0 eq.), dimethylamine HCl (1.09 g, 13.42 mmol, 1.5 eq.) and DIPEA (4.37 ml, 25.56 mmol, 4.0 eq.) in NMP (6.5 ml) was stirred for 1 hour at 130° C. in a microwave. The reaction mixture was diluted with water (100 ml) and extracted with ethyl acetate (2×150 ml). The combined org. phases were washed with sat. NaCl solution (200 ml), dried over sodium sulfate, concentrated under reduced pressure and purified by column chromatography (silica gel, 18% ethyl acetate in hexane). Yield: 78% (1.95 g, 7.01 mmol)

후처리

  1. extractionextracted with ethyl acetate (2×150 ml)
  2. washphases were washed with sat. NaCl solution (200 ml)
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. custompurified by column chromatography (silica gel, 18% ethyl acetate in hexane)

출처 및 근거

ORD 기록
ord-67eb56693b1d4a289e61b77b65fe6f2f
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08680159B2

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