Hydrochloric Acid → HCID 67916022、化合物

HRID 1029944ノート

反応式

HRID 1029944 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:8]2([C:23]3[CH:28]=[CH:27][CH:26]=[C:25]([Cl: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.Cl>O1CCOCC1.C(OC(C)C)(C)C>[ClH:1].[Cl:29][C:25]1[CH:24]=[C:23]([C:8]2([C:4]3[CH:5]=[CH:6][CH:7]=[C:2]([Cl: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

5

反応物 2

HCID 313Hydrochloric AcidHCID 67915885(3aRS,7aRS)-7,7-bis(3-chlorophenyl)-2-vinyloxycarbonylperhydro-4-isoindolone

生成物 1

HCID 67916022HCID 67916022、化合物収率 144.6%

試薬・触媒・溶媒 2

HCID 7914Diisopropyl Ether溶媒HCID 312751,4-Dioxane溶媒

反応条件

温度
60 °C

実験手順

(3aRS,7aRS)-7,7-bis-(3-chlorophenyl)-2-vinyloxycarbonyl-4-perhydroisoindolone (1.5 g) is treated with a 6N solution (7.4 cc) of hydrochloric acid in dioxane for 2 hours at 25° C. The solution is concentrated to dryness under reduced pressure (2.7 kPa) and the residue is heated for 1 hour in solution in ethanol at 60° C. and then stirred for 6 hours at 25° C. The solution is concentrated to dryness under reduced pressure (2.7 kPa) and the meringue obtained is solidified in isopropyl ether. The precipitate is drained and washed with isopropyl ether and then dried to give 7,7-bis-(3-chlorophenyl)-4-perhydroisoindolone hydrochloride (1 g).

後処理

  1. concentrationThe solution is concentrated to dryness under reduced pressure (2.7 kPa)
  2. concentrationThe solution is concentrated to dryness under reduced pressure (2.7 kPa)
  3. customthe meringue obtained
  4. washwashed with isopropyl ether
  5. customdried

出典と根拠

ORDレコード
ord-df257deec7c846ceacddc2f1551cf0d4
出典データセット
uspto-grants-1992_04
特許番号
US05102667

反応ノート

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