HCID 14625291, 화합물 → HCID 14517660, 화합물

HRID 2352453노트

반응식

HRID 2352453 반응식
[Cl:1][C:2]1[N:3]([C:11]2[CH:16]=[C:15]([N+:17]([O-])=O)[C:14]([O:20][CH2:21][C:22](OCCCC)=[O:23])=[CH:13][C:12]=2[F:29])[N:4]=[C:5]2[C:10]=1[CH2:9][CH2:8][CH2:7][CH2:6]2>C(O)(=O)C.[Fe]>[Cl:1][C:2]1[N:3]([C:11]2[C:12]([F:29])=[CH:13][C:14]3[O:20][CH2:21][C:22](=[O:23])[NH:17][C:15]=3[CH:16]=2)[N:4]=[C:5]2[C:10]=1[CH2:9][CH2:8][CH2:7][CH2:6]2

참가 물질

4

반응물 1

HCID 14625291HCID 14625291, 화합물

생성물 1

HCID 14517660HCID 14517660, 화합물수율 82.1%

시약·촉매·용매 2

HCID 23925Iron촉매HCID 176Acetic Acid용매

실험 절차

A suspension of 3-chloro-2-(2-fluoro-4-butyloxycarbonylmethoxy-5-nitrophenyl)-4,5,6,7-tetrahydro-2H-indazole (10 g) and iron powders (10 g) in acetic acid was refluxed for 5 hours. After completion of the reaction, the reaction mixture was filtered by the use of celite, and the filtrate was combined with water and extracted with ethyl acetate. The oragnic layer was concentrated, and the residue was purified by column chromatography using a mixture of hexane and ethyl acetate as an eluent to give 3-chloro-2-[7-fluoro-2H-1,4-benzoxazine-3(4H)-on-6-yl]-4,5,6,7-tetrahydro-2H-indazole (6.2 g). nD29.0 1.5628.

후처리

  1. temperaturewas refluxed for 5 hours
  2. customAfter completion of the reaction
  3. filtrationthe reaction mixture was filtered by the use of celite
  4. extractionextracted with ethyl acetate
  5. concentrationThe oragnic layer was concentrated
  6. customthe residue was purified by column chromatography
  7. additiona mixture of hexane and ethyl acetate as an eluent

출처 및 근거

ORD 기록
ord-631a9f9bbfd746e4bb1f8c84f9e16a41
출처 데이터셋
uspto-grants-1989_10
특허 번호
US04877444

반응 노트

불러오는 중…