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Triethylamine → HCID 90280212, 화합물

HRID 1506651
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HRID 1506651 반응식
[OH:1][N:2]=[C:3](Cl)/[CH:4]=[CH:5]\[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[Cl:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]#[CH:21])=[CH:16][CH:15]=1.C(N(CC)CC)C>C[C]1[C](C)[C](C)[C](C)[C]1C.C1CC=CCCC=C1.Cl[Ru]>[Cl:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]2[C:3](/[CH:4]=[CH:5]/[C:6]3[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=3)=[N:2][O:1][CH:21]=2)=[CH:16][CH:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 70118Benzene, 1-chloro-4-ethynyl-HCID 90280186HCID 90280186, 화합물

생성물 1

HCID 90280212HCID 90280212, 화합물

시약·촉매·용매 1

HCID 178420236HCID 178420236, 화합물촉매

실험 절차

A screw-top Schlenk flask (250 mL) purged with dry nitrogen was charged with compound 25B (7.31 g, 40 mmol) and 4-chlorophenylacetylene (5.0 g, 36.6 mmol). At room temperature, degassed 1,2-dichloroethane (100 mL) was added followed by [Cp*RuCl(cod)] (450 mg, 1.18 mmol) and triethylamine (6.38 mL, 45.8 mmol). The flask was purged with N2 and capped. After being stirred at room temperature for 7 h, the reaction mixture was passed through a plug of silica gel, and washed with DCM. The resulting solution was concentrated and the residue was purified by column chromatography on silica gel (pure hexanes to 10:1 hexanes/EtOAc) to provide the desired compound. MS (m/z) 282.0 [M+H]+.

후처리

  1. customA screw-top Schlenk flask (250 mL) purged with dry nitrogen
  2. customAt room temperature, degassed 1,2-dichloroethane (100 mL)
  3. additionwas added
  4. customThe flask was purged with N2
  5. customcapped
  6. washwashed with DCM
  7. concentrationThe resulting solution was concentrated
  8. customthe residue was purified by column chromatography on silica gel (pure hexanes to 10:1 hexanes/EtOAc)

출처 및 근거

ORD 기록
ord-ac0191918bcb4ae2a7dc8c00f62c67b0
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09220710B2

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