1-Butyl-3-methylimidazolium hexafluorophosphate → Aminocyclotridec-11-en-2-one

HRID 354229

반응식

HRID 354229 반응식
[C:1]([N-]CC=C)(=[O:12])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9]C=C.F[P-](F)(F)(F)(F)F.C[N+]1C=C[N:27]([CH2:30][CH2:31][CH2:32][CH3:33])C=1>C(C1C=CC=C(C(C)C)C=1N=CC1C=C([N+]([O-])=O)C=CC=1[O-])(C)C.C(=[Ru+]Cl)C1C=CC=CC=1.C1(P(C2CCCCC2)C2CCCCC2)CCCCC1>[NH2:27][CH:30]1[CH2:31][CH:32]=[CH:33][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][C:1]1=[O:12]

참가 물질

4

반응물 2

HCID 27341741-Butyl-3-methylimidazolium hexafluorophosphateHCID 178443346HCID 178443346, 화합물

생성물 1

HCID 57144930Aminocyclotridec-11-en-2-one수율 80%

시약·촉매·용매 1

HCID 178420536HCID 178420536, 화합물촉매

실험 절차

58 mg (0.25 mmol) of 10-undecenoyl-allylamide and 10 mg of (tricyclohexylphosphine)-benzylidene-chloro-ruthenium-(IV) 2-[(2,6-diisopropylphenyl)imino]methyl-4-nitro-phenoxide (5 mol %) were dissolved in 3 g of 1-methyl-3-butylimidazolium hexafluorophosphate. The mixture was allowed to react at 40° C. for 14 hours. The ionic phase was extracted with dichloromethane. After filtration through a very short silica gel column (length about 0.5 cm), about 80% of the desired product were obtained (yield determined by means of gas chromatography). The trans/cis ratio of the product is about 5:1.

후처리

  1. customto react at 40° C. for 14 hours
  2. extractionThe ionic phase was extracted with dichloromethane
  3. filtrationAfter filtration through a very short silica gel column (length about 0.5 cm)

출처 및 근거

ORD 기록
ord-d1b2560460874b37961cc2a3d21bd241
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06756500B1

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