Diisopropylethylamine → HCID 67342449、化合物

HRID 451511

反応式

HRID 451511 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 67342449HCID 67342449、化合物収率 76.4%

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-97a5cba06aba46a4b17d85304e4b67f4
出典データセット
uspto-grants-2013_07
特許番号
US08486967B2

関連ノート

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