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Hydrochloric Acid → HCID 75288490, 화합물

HRID 1430751
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HRID 1430751 반응식
[CH:1]12[O:10][CH:7]([CH:8]=[CH:9]1)[CH:6]1[CH:2]2[C:3](=[O:12])[CH2:4][C:5]1=[O:11].C([O-])(=O)C.C([O-])(=O)C.C([O-])(=O)C.[Cl:25][C:26]1[CH:40]=[CH:39][C:29]([C:30]2[CH:31]=[CH:32][C:33]([CH2:37][CH3:38])=[C:34]([Pb+3])[CH:35]=2)=[CH:28][CH:27]=1.C(Cl)(Cl)Cl.Cl>CN(C)C1C=CN=CC=1.C(OCC)(=O)C>[Cl:25][C:26]1[CH:40]=[CH:39][C:29]([C:30]2[CH:35]=[CH:34][C:33]([CH2:37][CH3:38])=[C:32]([CH:4]3[C:3](=[O:12])[CH:2]4[CH:6]([CH:7]5[O:10][CH:1]4[CH:9]=[CH:8]5)[C:5]3=[O:11])[CH:31]=2)=[CH:28][CH:27]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 6212ChloroformHCID 2067932010-Oxa-tricyclo[5.2.1.0*2,6*]dec-8-ene-3,5-dioneHCID 178476534HCID 178476534, 화합물

생성물 1

HCID 75288490HCID 75288490, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매
HCID 8857Ethyl Acetate용매

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온도
40 °C

실험 절차

To a mixture of (1RS,2SR,6RS,7SR)-10-oxatricyclo[5.2.1.02,6]dec-8-ene-3,5-dione (1.7 g, 0.01 mol), 4-dimethylaminopyridine (5.0 g, 0.04 mol) and 4′-chloro-4-ethylbiphen-3-yllead triacetate (9.2 g, 0.015 mol) under an atmosphere of nitrogen is added dry chloroform (50 ml)). The reaction mixture is heated at 40° C. for 5 hours, then cooled to room temperature. The mixture is diluted with ethyl acetate (50 ml), acidified with 2N aqueous hydrochloric acid (50 ml), and the mixture is filtered to remove solids. The filtrate is poured into a separating funnel and extracted with ethyl acetate. The organic extracts are combined, dried over anhydrous magnesium sulfate, filtered and the filtrate is evaporated under reduced pressure. The crude product is purified by column chromatography on silica gel to give (1RS,2SR,6RS,7SR)-4-(4′-chloro-4-ethylbiphen-3-yl)-10-oxatricyclo[5.2.1.02,6]dec-8-ene-3,5-dione.

후처리

  1. temperaturecooled to room temperature
  2. filtrationthe mixture is filtered
  3. customto remove solids
  4. additionThe filtrate is poured into a separating funnel
  5. extractionextracted with ethyl acetate
  6. dry with materialdried over anhydrous magnesium sulfate
  7. filtrationfiltered
  8. customthe filtrate is evaporated under reduced pressure
  9. customThe crude product is purified by column chromatography on silica gel

출처 및 근거

ORD 기록
ord-dacd2030ac6149f7b132a0e0216b196a
출처 데이터셋
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08940913B2

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