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1,2-Dimethoxyethane → HCID 59496831, 화합물

HRID 416990
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HRID 416990 반응식
[CH2:1]([O:3][C:4](=[O:39])[CH2:5][CH2:6][CH2:7][O:8][C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][O:21][C:22]2[CH:27]=[C:26]([O:28][CH2:29][CH3:30])[CH:25]=[C:24](Br)[CH:23]=2)[C:10]=1[CH2:32][CH2:33][C:34]([O:36][CH2:37][CH3:38])=[O:35])[CH3:2].[C:40]1(B(O)O)[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=1.C(=O)([O-])[O-].[Cs+].[Cs+].C(COC)OC>C(OCC)(=O)C.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2]>[CH2:1]([O:3][C:4](=[O:39])[CH2:5][CH2:6][CH2:7][O:8][C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][O:21][C:22]2[CH:23]=[C:24]([C:40]3[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=3)[CH:25]=[C:26]([O:28][CH2:29][CH3:30])[CH:27]=2)[C:10]=1[CH2:32][CH2:33][C:34]([O:36][CH2:37][CH3:38])=[O:35])[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 80711,2-DimethoxyethaneHCID 10796Cesium carbonateHCID 66827Phenylboronic AcidHCID 59496797HCID 59496797, 화합물

생성물 1

HCID 59496831HCID 59496831, 화합물수율 84.3%

시약·촉매·용매 2

HCID 44119782
Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)
촉매
HCID 8857Ethyl Acetate용매

반응 조건

온도
120 °C

실험 절차

To a mixture of 4-[3-[6-(3-bromo-5-ethoxy-phenoxy)-hexyl]-2-(2-ethoxycarbonyl-ethyl)-phenoxy]-butyric acid ethyl ester (305 mg, 0.5 mmol), phenylboronic acid (125 mg, 1.0 mmol), [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) (55 mg, 0.075 mmol), and cesium carbonate (331 mg, 1.0 mmol) in a microwave tube was added dimethoxyethane (5.9 mL) under nitrogen atmosphere at room temperature. The resulting brown reaction mixture was heated to 120° C. in a microwave for 30 minutes. The reaction mixture was diluted with ethyl acetate (50 mL) and the undissolved residue was filtered off and washed with water (50 mL). Then, the two layers of filtrate were separated and the aqueous layer was extracted with ethyl acetate (20 mL). The combined organic extracts were washed with water (50 mL) and brine solution (50 mL). The organic layer was dried over anhydrous magnesium sulfate and filtration of the drying agent and removal of the solvent under vacuum gave the colored residue which was purified by using an ISCO 40 column, eluting with 2-25% ethyl acetate in hexanes to obtain 4-[3-[6-(5-ethoxy-biphenyl-3-yloxy)-hexyl]-2-(2-ethoxycarbonyl-ethyl)-phenoxy]-butyric acid ethyl ester (255 mg, 84%) as a colorless viscous oil: ES(+)-LRMS m/e calcd for C37H48O7 (M+Na)+ 627.3292. found 627.3292.

후처리

  1. filtrationthe undissolved residue was filtered off
  2. washwashed with water (50 mL)
  3. customThen, the two layers of filtrate were separated
  4. extractionthe aqueous layer was extracted with ethyl acetate (20 mL)
  5. washThe combined organic extracts were washed with water (50 mL) and brine solution (50 mL)
  6. dry with materialThe organic layer was dried over anhydrous magnesium sulfate and filtration of the drying agent and removal of the solvent under vacuum
  7. customgave the colored residue which
  8. customwas purified
  9. washeluting with 2-25% ethyl acetate in hexanes

출처 및 근거

ORD 기록
ord-f462e84033e04b18a1fdc97c782e5ef5
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08088936B2

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