HCID 86631214、化合物 → HCID 86631215、化合物

HRID 253017

反応式

HRID 253017 の反応式
C=[C:2]([CH2:26][CH2:27][CH3:28])[CH2:3][CH2:4][N:5]([C@@H:18]([CH2:23][CH:24]=C)[C:19]([O:21][CH3:22])=[O:20])[S:6]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[N+:15]([O-:17])=[O:16])(=[O:8])=[O:7]>C(Cl)Cl.CC1C=C(C)C(N2C(=[Ru](Cl)(Cl)=CC3C=CC=CC=3)N(C3C(C)=CC(C)=CC=3C)CC2)=C(C)C=1.C1CCC(P(C2CCCCC2)C2CCCCC2)CC1>[N+:15]([C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=1[S:6]([N:5]1[CH2:4][CH2:3][C:2]([CH2:26][CH2:27][CH3:28])=[CH:24][CH2:23][C@H:18]1[C:19]([O:21][CH3:22])=[O:20])(=[O:8])=[O:7])([O-:17])=[O:16]

参加物

4

反応物 1

HCID 86631214HCID 86631214、化合物

生成物 1

HCID 86631215HCID 86631215、化合物収率 82%

試薬・触媒・溶媒 2

HCID 11147261(1,3-Dimesitylimidazolidin-2-ylidene)(tricyclohexylphosphine)benzylidene ruthenium dichloride触媒HCID 6344Dichloromethane溶媒

実験手順

Benzylidene[1,3-bis(2,4,6-trimethylphenyl)-2-imidazolidinylidene]dichloro(tricyclohexylphosphine)ruthenium (250 mg, 0.295 mmol) was added to a solution of 2.42 g (5.89 mmol) of the title compound produced in step (iii) of Example 47 in methylene chloride (295 ml), and the mixture was heated under reflux for one hr. The reaction solution was cooled to room temperature, and the solvent was removed under the reduced pressure. The residue was purified by column chromatography on silica gel (hexane:ethyl acetate=10:1) to give 1.84 g (yield 82%) of the title compound.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for one hr
  3. customthe solvent was removed under the reduced pressure
  4. customThe residue was purified by column chromatography on silica gel (hexane:ethyl acetate=10:1)

出典と根拠

ORDレコード
ord-0e8c165c80d44013a534d4718e2784c2
出典データセット
uspto-grants-2011_01
特許番号
US07871982B2

関連ノート

読み込み中…