Ethanol → HCID 67346936, 화합물

HRID 1842596

반응식

HRID 1842596 반응식
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

참가 물질

6

반응물 4

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

생성물 1

HCID 67346936HCID 67346936, 화합물수율 80.8%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
70 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-d2d13dc2b371450b93e0b6e18f022f55
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08946237B2

연결된 노트

불러오는 중…