Diisopropylethylamine → HCID 67342449, 화합물

HRID 451511

반응식

HRID 451511 반응식
IC1C=[CH:6][N:5]=[C:4]([C:8]([F:11])([F:10])[F:9])C=1.[C:12]([N:19]1CCC(N)C[CH2:20]1)([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13].[CH3:26][CH2:27][N:28]([CH:32]([CH3:34])[CH3:33])[CH:29]([CH3:31])C>CN1C(=O)CCC1>[F:11][C:8]([F:9])([F:10])[C:4]1[CH:33]=[C:32]([N:28]2[CH2:27][CH2:26][CH:20]([NH:19][C:12](=[O:13])[O:14][C:15]([CH3:18])([CH3:17])[CH3:16])[CH2:31][CH2:29]2)[CH:34]=[CH:6][N:5]=1

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 12682914-Amino-1-Boc-piperidineHCID 234369404-Iodo-2-(trifluoromethyl)pyridine

생성물 1

HCID 67342449HCID 67342449, 화합물수율 76.4%

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

To a mixture of 4-iodo-2-(trifluoromethyl)pyridine (356 mg, 1.3 mmol) and Boc-4-aminopiperidine (340 mg, 1.7 mmol) in NMP (2.6 mL) was added DIPEA (319 L, 1.83 mmol). Argon was bubbled through the cloudy solution for 5 minutes before the reaction mixture was heated in the microwave for 3×30 minutes to 150° C. The mixture was then poured into water and extracted with ethyl acetate. The combined organic phases were dried over sodium sulfate, filtered and evaporated. Purification by chromatography (silica gel, 50 g, 0 to 100% ethyl acetate in heptane) afforded the title compound (343 mg, 76%) as a white solid.

후처리

  1. customArgon was bubbled through the cloudy solution for 5 minutes before the reaction mixture
  2. temperaturewas heated in the microwave for 3×30 minutes to 150° C
  3. additionThe mixture was then poured into water
  4. extractionextracted with ethyl acetate
  5. dry with materialThe combined organic phases were dried over sodium sulfate
  6. filtrationfiltered
  7. customevaporated
  8. customPurification by chromatography (silica gel, 50 g, 0 to 100% ethyl acetate in heptane)

출처 및 근거

ORD 기록
ord-97a5cba06aba46a4b17d85304e4b67f4
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08486967B2

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