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

HRID 1196241ノート

反応式

HRID 1196241 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
60 °C

実験手順

(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.

後処理

  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

出典と根拠

ORDレコード
ord-73dc76b3cdb84a54af2dc93b924c4251
出典データセット
uspto-grants-1992_05
特許番号
US05112988

反応ノート

読み込み中…