Hydrochloric Acid → HCID 46872043、化合物

HRID 336178

反応式

HRID 336178 の反応式
[C:1]([C:5]1[O:9][N:8]=[C:7]([NH:10][C:11]([CH:13]2[CH2:18][CH2:17][CH2:16][NH:15][CH2:14]2)=[O:12])[CH:6]=1)([CH3:4])([CH3:3])[CH3:2].Cl.[Cl:20][C:21]1[C:22](F)=[N:23][CH:24]=[C:25]([C:27]([F:30])([F:29])[F:28])[CH:26]=1.C(N(CC)CC)C>C(O)(C)(C)C>[C:1]([C:5]1[O:9][N:8]=[C:7]([NH:10][C:11]([CH:13]2[CH2:18][CH2:17][CH2:16][N:15]([C:22]3[C:21]([Cl:20])=[CH:26][C:25]([C:27]([F:30])([F:28])[F:29])=[CH:24][N:23]=3)[CH2:14]2)=[O:12])[CH:6]=1)([CH3:4])([CH3:2])[CH3:3]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 12680753-Chloro-2-fluoro-5-(trifluoromethyl)pyridineHCID 58563805HCID 58563805、化合物

生成物 1

HCID 46872043HCID 46872043、化合物

試薬・触媒・溶媒 1

HCID 6386tert-Butanol溶媒

反応条件

温度
175 °C

実験手順

A microwave reaction vial is charged with piperidine-3-carboxylic acid (5-tert-butyl-isoxazol-3-yl)-amide; hydrochloride (94 mg; 0.327 mmol), 3-chloro-2-fluoro-5-trifluoromethylpyridine (0.043 mL; 0.33 mmol), triethylamine (0.092 mL; 0.66 mmol) and t-butanol (0.5 mL). The vial is heated in microwave at 175° C. for 1 hour then left standing at room temperature overnight. The reaction mixture is concentrated in vacuo. Purification by flash chromatography on silica using methanol/methylene chloride then recrystallization from hot methanol provides the title compound, m/z 431 [M+H+].

後処理

  1. customA microwave reaction
  2. waitthen left
  3. concentrationThe reaction mixture is concentrated in vacuo
  4. customPurification by flash chromatography on silica
  5. customrecrystallization from hot methanol

出典と根拠

ORDレコード
ord-b7d621c0d7a44d1389355d608ad1b156
出典データセット
uspto-grants-2014_11
特許番号
US08889670B2

関連ノート

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