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

HRID 1196241노트

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HRID 1196241 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-vinyloxycarbonylperhydro-4-isoindolone (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 taken up with ethanol (500 cc). The solution is heated to 60° C. for 6 hours and stirred for 16 hours at 25° C., then concentrated to one half under reduced pressure (2.7 kPa), and the crystals formed are drained and washed with isopropyl ether, then dried. 7,7-Bis(3-fluorophenyl)perhydro-4-isoindolone 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 one half under reduced pressure (2.7 kPa)
  3. customthe crystals formed
  4. washwashed with isopropyl ether
  5. customdried

출처 및 근거

ORD 기록
ord-73dc76b3cdb84a54af2dc93b924c4251
출처 데이터셋
uspto-grants-1992_05
특허 번호
US05112988

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