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Tetrahydrofuran → (E)-3-{8-(4-fluoro-3-methylphenyl)-10,10-dimethyl-1,5dithiaspiro{5.5}undec-8-en-9-yl}propenal

HRID 2165135
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인쇄 미리보기

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HRID 2165135 반응식
[Li+].CC([N-]C(C)C)C.C(=NC1CCCCC1)C.[F:18][C:19]1[CH:24]=[CH:23][C:22]([C:25]2[CH2:26][C:27]3([CH2:33][C:34]([CH3:39])([CH3:38])[C:35]=2C=O)[S:32][CH2:31][CH2:30][CH2:29][S:28]3)=[CH:21][C:20]=1[CH3:40].[CH2:41]1C[O:44][CH2:43][CH2:42]1>CCOCC>[F:18][C:19]1[CH:24]=[CH:23][C:22]([C:25]2[CH2:26][C:27]3([CH2:33][C:34]([CH3:38])([CH3:39])[C:35]=2/[CH:41]=[CH:42]/[CH:43]=[O:44])[S:28][CH2:29][CH2:30][CH2:31][S:32]3)=[CH:21][C:20]=1[CH3:40]
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참가 물질

6

반응물 4

HCID 8028TetrahydrofuranHCID 2724682Lithium diisopropylamideHCID 10964544N-cyclohexylethanimineHCID 150569548-(4-Fluoro-3-methylphenyl)-10,10-dimethyl-1,5dithiaspiro{5.5}undec-8-en-9-carboxaldehyde

생성물 1

HCID 15056955(E)-3-{8-(4-fluoro-3-methylphenyl)-10,10-dimethyl-1,5dithiaspiro{5.5}undec-8-en-9-yl}propenal

시약·촉매·용매 1

HCID 3283
Diethyl Ether
용매

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온도
-78 °C

실험 절차

To a -20° C. solution of LDA (19.0 mmol) in 60 mL anhydrous THF was added ethylidenecyclohexylamine (Org. Syn. 50, 66) (2.38 gm, 19.0 mmol). The solution was stirred for 30 min, cooled to -78° C. and a solution of 8 (3.50 g, 10.0 mmol) in 60 mL was added. The mixture was stirred for 3 h, diluted with ether and quenched with H2O. The organic layer was washed with H2O and brine and dried (MgSO4). Removal of the volatiles in vacuo and purification of the residue by HPLC using 10:1 hexanes:EtOAc provided 1.6 g of the orange color gum.

후처리

  1. stirringThe mixture was stirred for 3 h
  2. customquenched with H2O
  3. washThe organic layer was washed with H2O and brine
  4. dry with materialdried (MgSO4)
  5. customRemoval of the volatiles
  6. customin vacuo and purification of the residue by HPLC
  7. customEtOAc provided 1.6 g of the orange color gum

출처 및 근거

ORD 기록
ord-ab7e5118937246dc943924729c27e232
출처 데이터셋
uspto-grants-1990_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04939143

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