HCID 86655969, 화합물 → HCID 86655968, 화합물

HRID 626638

반응식

HRID 626638 반응식
[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

참가 물질

5

반응물 1

HCID 86655969HCID 86655969, 화합물

생성물 1

HCID 86655968HCID 86655968, 화합물수율 73.2%

시약·촉매·용매 3

HCID 11147261(1,3-Dimesitylimidazolidin-2-ylidene)(tricyclohexylphosphine)benzylidene ruthenium dichloride촉매HCID 178425456HCID 178425456, 화합물촉매HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-bb6be0ca53ed4ae6891a7462896bf134
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09309207B2

연결된 노트

불러오는 중…