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

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.

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

ORDレコード

ord-2c745b4e9ef04c778705040fece993af

出典データセット

uspto-grants-2013_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08563582B2