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Pyridine → 3,4-Dihydro-2h-pyran-2-ylmethyl acetate

HRID 249666
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HRID 249666 반응식
[O:1]1[CH:6]=[CH:5][CH2:4][CH2:3][CH:2]1[CH2:7][OH:8].[C:9](OC(=O)C)(=[O:11])[CH3:10].N1C=CC=CC=1>C(OCC)(=O)C>[C:9]([O:8][CH2:7][CH:2]1[CH2:3][CH2:4][CH:5]=[CH:6][O:1]1)(=[O:11])[CH3:10]
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참가 물질

5

반응물 3

HCID 1049PyridineHCID 7918Acetic AnhydrideHCID 955593,4-dihydro-2H-pyran-2-methanol

생성물 1

HCID 2281263,4-Dihydro-2h-pyran-2-ylmethyl acetate수율 86%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

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온도
0 °C

실험 절차

A mixture of (±)-3,4-dihydro-2H-pyran-2-methanol (514 g, 4.51 mol, 1 eq) and acetic anhydride (621 g, 6.09 mol, 1.35 eq) was cooled to 0° C. To the resultant mixture was added pyridine (35.6 g, 0.45 mol, 0.1 eq) and the resultant reaction mixture was allowed to warm to room temperature with stirring. The resultant reaction mixture was allowed to stir for an additional 8 hours after reaching room temperature and was shown to be complete by thin-layer chromatography (2:1 hexanes:ethyl acetate, 12 staining). The reaction mixture was concentrated in vacuo at 35° C. and the resultant residue was diluted using ethyl acetate (2 L). The resultant mixture was transferred to a separatory funnel and sequentially washed with deionized water (3×1 L), saturated aqueous NaHCO3 (2×10 L), and brine (1.0 L). The organic layer was dried over sodium sulfate and concentrated in vacuo at 35° C. to provide (±)-3,4-dihydro-2H-pyran-2-yl-methyl acetate as a clear liquid (605.9 g, 86% yield). 1H NMR (300 MHz, CDCl3) δ 1.6-2.2 (m, 4 H), 2.1 (s, 3 H), 4.2 (m, 3 H), 4.8 (m, 1 H), 6.4 (m, 1 H).

후처리

  1. customthe resultant reaction mixture
  2. temperatureto warm to room temperature
  3. customThe resultant reaction mixture
  4. stirringto stir for an additional 8 hours
  5. customafter reaching room temperature
  6. concentrationThe reaction mixture was concentrated in vacuo at 35° C.
  7. additionthe resultant residue was diluted
  8. customThe resultant mixture was transferred to a separatory funnel
  9. washsequentially washed with deionized water (3×1 L), saturated aqueous NaHCO3 (2×10 L), and brine (1.0 L)
  10. dry with materialThe organic layer was dried over sodium sulfate
  11. concentrationconcentrated in vacuo at 35° C.

출처 및 근거

ORD 기록
ord-f1303610e2ac404895f42a2ff879fd77
출처 데이터셋
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07863253B2

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