Phosgene → HCID 20450024, 화합물

HRID 358061노트

반응식

HRID 358061 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]=[C:10]([NH:12][NH2:13])[CH2:9][CH:8]=[C:7]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=3[F:20])[C:6]=2[CH:21]=1.[C:22](Cl)(Cl)=[O:23]>N1C=CC=CC=1.C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]3[C:22](=[O:23])[NH:13][N:12]=[C:10]3[CH2:9][CH:8]=[C:7]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=3[F:20])[C:6]=2[CH:21]=1

참가 물질

5

반응물 2

HCID 6371PhosgeneHCID 20449973HCID 20449973, 화합물

생성물 1

HCID 20450024HCID 20450024, 화합물

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 1140Toluene용매

실험 절차

0.15 g of 7-chloro-5-(2-fluorophenyl)-2-hydrazino-3H-1-benzazepine is dissolved in 10 ml of pyridine and treated with 1.44 ml of a 14.3% solution of phosgene in toluene. The mixture is heated to 60° for 5 minutes and then evaporated in vacuo. The residue is partitioned between benzene and water. The benzene phase is washed successively with water, with sodium hydrogen carbonate solution and with water. The solvent is evaporated in vacuo. The residue is chromatographed on 15 g of silica gel while eluting with benzene/ethyl acetate (19:1 and 9:1). After recrystallization from ether/hexane, there is obtained pure 8-chloro-6-(2-fluorophenyl)-2,4-dihydro-1H-s-triazolo[4,3-a][1]benzazepin-1-one of melting point 223°-225°.

후처리

  1. temperatureThe mixture is heated to 60° for 5 minutes
  2. customevaporated in vacuo
  3. customThe residue is partitioned between benzene and water
  4. washThe benzene phase is washed successively with water, with sodium hydrogen carbonate solution and with water
  5. customThe solvent is evaporated in vacuo
  6. customThe residue is chromatographed on 15 g of silica gel
  7. washwhile eluting with benzene/ethyl acetate (19:1 and 9:1)
  8. customAfter recrystallization from ether/hexane

출처 및 근거

ORD 기록
ord-6b4689f3149c44fa96782260fb471bcb
출처 데이터셋
uspto-grants-1984_08
특허 번호
US04464300

반응 노트

불러오는 중…