HCID 86655969、化合物 → HCID 86655968、化合物

HRID 626638

反応式

HRID 626638 の反応式
[CH2:1]([O:8][C:9](=[O:33])[NH:10][C@@H:11]([C:21](=[O:32])[NH:22][C@H:23]([CH2:27][O:28][CH2:29][CH:30]=C)[CH:24]([CH3:26])[CH3:25])[CH2:12][C:13]1[N:14]=[CH:15][N:16]([CH2:18][CH:19]=C)[CH:17]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>ClCCl.Cl[Ru](=C1N(C2C(C)=CC(C)=CC=2C)CCN1C1C(C)=CC(C)=CC=1C)(Cl)(=CC1C=CC=CC=1)[P](C1CCCCC1)(C1CCCCC1)C1CCCCC1>[CH2:1]([O:8][C:9](=[O:33])[NH:10][C@@H:11]1[CH2:12][C:13]2=[CH:17][N:16]([CH:15]=[N:14]2)[CH2:18][CH:19]=[CH:30][CH2:29][O:28][CH2:27][C@H:23]([CH:24]([CH3:25])[CH3:26])[NH:22][C:21]1=[O:32])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 1

HCID 86655969HCID 86655969、化合物

生成物 1

HCID 86655968HCID 86655968、化合物収率 73.2%

試薬・触媒・溶媒 3

HCID 11147261(1,3-Dimesitylimidazolidin-2-ylidene)(tricyclohexylphosphine)benzylidene ruthenium dichloride触媒HCID 178425456HCID 178425456、化合物触媒HCID 6344Dichloromethane溶媒

実験手順

A solution of 0.735 g (1.62 mmol) of benzyl[(R)-2-(1-allyl-1H-imidazol-4-yl)-1-((S)-1-allyloxymethyl-2-methylpropylcarbamoyl)ethyl]carbamate in 370 ml of dichloromethane was mixed with 0.210 g (0.24 mmol) of benzylidene[1,3-bis(2,4,6-trimethylphenyl)-2-imidazolidinylidene]dichloro(tricyclohexylphosphine)ruthenium (Grubbs II catalyst) and stirred at RT. The mixture was stirred at RT for several days with repeated addition of Grubbs II catalyst until starting material was no longer present (LC/MS). The mixture was concentrated and the residue was chromatographed on silica gel (dichloromethane/methanol 99:1→9:1). 0.506 g of the title compound was obtained.

後処理

  1. stirringThe mixture was stirred at RT for several days
  2. concentrationThe mixture was concentrated
  3. customthe residue was chromatographed on silica gel (dichloromethane/methanol 99:1→9:1)

出典と根拠

ORDレコード
ord-bb6be0ca53ed4ae6891a7462896bf134
出典データセット
uspto-grants-2016_04
特許番号
US09309207B2

関連ノート

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