Hydrochloric Acid → 7,7-Bis(3-Fluorophenyl)-4-perhydroisoindolone hydrochloride

HRID 1029933노트

반응식

HRID 1029933 반응식
[F:1][C:2]1[CH:3]=[C:4]([C:8]2([C:23]3[CH:28]=[CH:27][CH:26]=[C:25]([F:29])[CH:24]=3)[CH:16]3[CH:12]([CH2:13][N:14](C(OC=C)=O)[CH2:15]3)[C:11](=[O:22])[CH2:10][CH2:9]2)[CH:5]=[CH:6][CH:7]=1.[ClH:30]>O1CCOCC1>[ClH:30].[F:29][C:25]1[CH:24]=[C:23]([C:8]2([C:4]3[CH:5]=[CH:6][CH:7]=[C:2]([F:1])[CH:3]=3)[CH:16]3[CH:12]([CH2:13][NH:14][CH2:15]3)[C:11](=[O:22])[CH2:10][CH2:9]2)[CH:28]=[CH:27][CH:26]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 67916103(3aRS,7aRS)-7,7-bis(3-fluorophenyl)-2-vinyloxycarbonylperhydro-4-isoindolone

생성물 1

HCID 679158007,7-Bis(3-Fluorophenyl)-4-perhydroisoindolone hydrochloride

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
60 °C

실험 절차

(3aRS,7aRS)-7,7-bis-(3-fluorophenyl)-2-vinyloxycarbonyl-4-perhydroisoindolone (64.5 g) is treated with a 6N solution (330 cc) of hydrochloric acid in dioxane for 30 minutes at 25° C. The solution is concentrated to dryness under reduced pressure (2.7 kPa) and the residue is taken up in ethanol (500 cc). The solution is heated at 60° C. for 6 hours and stirred for 16 hours at 25° C. and then concentrated to half its volume under reduced pressure (2.7 kPa) and the crystals formed are drained and washed with isopropyl ether and then dried. 7,7-Bis(3-Fluorophenyl)-4-perhydroisoindolone hydrochloride (48.7 g) is obtained. m.p.=264° C.

후처리

  1. concentrationThe solution is concentrated to dryness under reduced pressure (2.7 kPa)
  2. concentrationconcentrated to half its volume under reduced pressure (2.7 kPa)
  3. customthe crystals formed
  4. washwashed with isopropyl ether
  5. customdried

출처 및 근거

ORD 기록
ord-f6ef978905854ab89d11991531b4a5e1
출처 데이터셋
uspto-grants-1992_04
특허 번호
US05102667

반응 노트

불러오는 중…