Methanol → 4,4-Dimethoxytetrahydro-2H-pyran-3-ol

HRID 1436747

반응식

HRID 1436747 반응식
[CH3:1][O:2][C:3]1[CH2:4][CH2:5][O:6][CH2:7][CH:8]=1.ClC1C=CC=C([C:16](OO)=[O:17])C=1.C[OH:21]>>[CH3:1][O:2][C:3]1([O:17][CH3:16])[CH2:4][CH2:5][O:6][CH2:7][CH:8]1[OH:21]

참가 물질

4

반응물 3

HCID 887Methanol2회HCID 70297m-Chloroperbenzoic acidHCID 870513,6-dihydro-4-methoxy-2H-pyran

생성물 1

HCID 121909884,4-Dimethoxytetrahydro-2H-pyran-3-ol

실험 절차

To a solution of 4-methoxy-3,6-dihydro-2H-pyran (5.00 g, 43.8 mmol) in methanol (100 mL) at 0° C. was dropwise added a solution of m-chloroperbenzoic acid (15.1 g, 87.6 mmol) in methanol (15 mL). After being stirred for 5 h, methanol was removed in vacuo and the white residue was dissolved in methylene chloride (300 mL). To the solution was added K2CO3. The resulting solution was stirred for 1 h and filtered through celite. The filtrate was evaporated in vacuo to provide the desired product which was used directly for the next reaction without purification.

후처리

  1. custommethanol was removed in vacuo
  2. dissolutionthe white residue was dissolved in methylene chloride (300 mL)
  3. additionTo the solution was added K2CO3
  4. stirringThe resulting solution was stirred for 1 h
  5. filtrationfiltered through celite
  6. customThe filtrate was evaporated in vacuo

출처 및 근거

ORD 기록
ord-a522f38e36d0493d8fee958960b0b03b
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07618970B2

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