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Tetrahydrofuran → 3-[Hydroxy-(4-triisopropylsilanyloxymethyl-phenyl)-methyl]-benzonitrile

HRID 1717711
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HRID 1717711 반응식
Br[C:2]1[CH:19]=[CH:18][C:5]([CH2:6][O:7][Si:8]([CH:15]([CH3:17])[CH3:16])([CH:12]([CH3:14])[CH3:13])[CH:9]([CH3:11])[CH3:10])=[CH:4][CH:3]=1.O1CCCC1.C([Li])CCC.[C:30]([C:32]1[CH:33]=[C:34]([CH:37]=[CH:38][CH:39]=1)[CH:35]=[O:36])#[N:31]>[Cl-].[NH4+].C(OCC)(=O)C>[OH:36][CH:35]([C:2]1[CH:19]=[CH:18][C:5]([CH2:6][O:7][Si:8]([CH:15]([CH3:17])[CH3:16])([CH:12]([CH3:14])[CH3:13])[CH:9]([CH3:11])[CH3:10])=[CH:4][CH:3]=1)[C:34]1[CH:33]=[C:32]([CH:39]=[CH:38][CH:37]=1)[C:30]#[N:31]
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참가 물질

7

반응물 4

HCID 8028Tetrahydrofuran2회HCID 90670m-FormylbenzonitrileHCID 11439315(4-Bromo-benzyloxy)-triisopropyl-silaneHCID 178418339Butyllithium

생성물 1

HCID 666996123-[Hydroxy-(4-triisopropylsilanyloxymethyl-phenyl)-methyl]-benzonitrile수율 75%

시약·촉매·용매 2

HCID 8857
Ethyl Acetate
용매
HCID 25517Ammonium Chloride용매

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온도
-78 °C

실험 절차

Stir a solution of (4-bromo-benzyloxy)-triisopropyl-silane (72 g, 209.7 mmol) and tetrahydrofuran (500 mL) at −78° C. Add a 1.6 M solution of n-butyllithium in hexanes (143 mL) over 10 min. After addition, allow the reaction mixture to reach −20° C. and stir for 5 minutes. Cool the reaction mixture to −78° C. In another flask, stir a solution of 3-cyanobenzaldehyde (25 g, 190.6 mmol) and tetrahydrofuran (250 mL) at −78° C. Add the lithium anion solution to the aldehyde solution via large canula at a rate such that the internal aldehyde temperature does not rise above −50° C. After addition is complete, stir the reaction mixture 18 hours at room temperature. Dilute the reaction mixture with aqueous saturated ammonium chloride (500 mL) and ethyl acetate (200 mL). Separate the layers, and extract the aqueous layer with ethyl acetate (3×100 mL). Combine the organic layers, dry over anhydrous magnesium sulfate, filter, and concentrate. Purify the residue via silica gel chromatography eluting with hexanes to 9:1 hexanes:ethyl acetate to afford the title compound (56.1 g, 75%) as a colorless oil. LCMS (m/z) 396 M+1.

후처리

  1. additionAfter addition
  2. customto reach −20° C.
  3. customdoes not rise above −50° C
  4. additionAfter addition
  5. stirringstir the reaction mixture 18 hours at room temperature
  6. customSeparate the layers
  7. extractionextract the aqueous layer with ethyl acetate (3×100 mL)
  8. dry with materialCombine the organic layers, dry over anhydrous magnesium sulfate
  9. filtrationfilter
  10. concentrationconcentrate
  11. customPurify the residue via silica gel chromatography
  12. washeluting with hexanes to 9:1 hexanes

출처 및 근거

ORD 기록
ord-a46e6483112643e696609ad9657141e1
출처 데이터셋
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07803938B2

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