4-(2-Chlorooxazol-5-yl)benzonitrile → HCID 178509592、化合物

HRID 537866

反応式

HRID 537866 の反応式
Cl[C:2]1[O:3][C:4]([C:7]2[CH:14]=[CH:13][C:10]([C:11]#[N:12])=[CH:9][CH:8]=2)=[CH:5][N:6]=1.[NH:15]1[C:19]([C:20]2[CH:21]=[C:22]([CH:24]=[CH:25][CH:26]=2)[NH2:23])=[N:18][N:17]=[N:16]1>CC(O)C>[NH:18]1[C:19]([C:20]2[CH:21]=[C:22]([NH:23][C:2]3[O:3][C:4]([C:7]4[CH:14]=[CH:13][C:10]([C:11]#[N:12])=[CH:9][CH:8]=4)=[CH:5][N:6]=3)[CH:24]=[CH:25][CH:26]=2)=[N:15][N:16]=[N:17]1

参加物

4

反応物 2

HCID 684435584-(2-Chlorooxazol-5-yl)benzonitrileHCID 178507542HCID 178507542、化合物

生成物 1

HCID 178509592HCID 178509592、化合物収率 100.6%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

反応条件

温度
80 °C

実験手順

A mixture of 4-(2-chlorooxazol-5-yl)benzonitrile 2 (0.216 g, 1.05 mmol) and commercially available 3-(1H-tetrazol-5-yl)aniline 35 (0.17 g, 1.05 mmol) in 2-propanol (20 mL) was heated to 80° C. for 18 h with stirring. Upon cooling, a white solid precipitated out which was filtered off, washed with 2-propanol, and dried. This was further purified by dissolving into DMSO and re-precipitated with addition of water. Resulting solid was filtered, washed with water, methanol and dried under high vacuum to yield 4-(2-((3-(1H-tetrazol-5-yl)phenyl)amino)oxazol-5-yl)benzonitrile 36 as a white solid (0.348 g, 100%). MS (ES) m/z 330 (M+H+).

後処理

  1. temperatureUpon cooling
  2. customa white solid precipitated out which
  3. filtrationwas filtered off
  4. washwashed with 2-propanol
  5. customdried
  6. customThis was further purified
  7. dissolutionby dissolving into DMSO
  8. customre-precipitated with addition of water
  9. customResulting solid
  10. filtrationwas filtered
  11. washwashed with water, methanol
  12. customdried under high vacuum

出典と根拠

ORDレコード
ord-1c09c89417e34647ab4c1efe2db7dede
出典データセット
uspto-grants-2014_10
特許番号
US08865709B2

関連ノート

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