Ethanol → HCID 67346936、化合物

HRID 1842596

反応式

HRID 1842596 の反応式
N#N.[NH2:3][C:4]1[C:8]([Br:9])=[CH:7][NH:6][N:5]=1.CN(/[CH:13]=[C:14](\[Cl:19])/[CH:15]=[N+](C)C)C.F[P-](F)(F)(F)(F)F.C(O)C>C(O)(=O)C>[Br:9][C:8]1[CH:7]=[N:6][N:5]2[CH:15]=[C:14]([Cl:19])[CH:13]=[N:3][C:4]=12

参加物

6

反応物 4

HCID 702EthanolHCID 947NitrogenHCID 105908072-Chloro-1,3-bis(dimethylamino)trimethinium hexafluorophosphateHCID 178509245HCID 178509245、化合物

生成物 1

HCID 67346936HCID 67346936、化合物収率 80.8%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
70 °C

実験手順

A 5 L 4-neck round bottom flask equipped with mechanical stirrer, thermocouple, condenser and N2 bubbler was charged with 3-amino-4-bromopyrazole (40.0 g, 240 mmol), 2-Chloro-1,3-bis(dimethylamino)trimethinium hexafluorophosphate (77.0 g, 252 mmol) in acetic acid (390 ml)/ethanol (580 ml). The reaction mixture was heated to 70° C. for 8 hrs. Cool to 0° C. Filter off solids. Wash solids with 500 ml water then 500 ml MeOH and dried under high vac to afford the title compound (45.1 g, 194 mmol). LRMS (APCI) calc'd for (C6H3BrClN3) [M+H]+, 231.9; found 231.9. 1H NMR (CDCl3, 500 MHz) δ 8.74 (s, 1H), 8.52 (s, 1H), 8.14 (s, 1H).

後処理

  1. customA 5 L 4-neck round bottom flask equipped with mechanical stirrer
  2. temperatureCool to 0° C
  3. filtrationFilter off solids
  4. washWash solids with 500 ml water
  5. dry with material500 ml MeOH and dried under high vac

出典と根拠

ORDレコード
ord-d2d13dc2b371450b93e0b6e18f022f55
出典データセット
uspto-grants-2015_02
特許番号
US08946237B2

関連ノート

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