Diethyl Ether → 3-Hydroxy-2,2-dimethyl-1-propylthiocyanate

A mixture of 16.7 g of 3-bromo-2,2-dimethyl-1-propanol, 14.6 g of potassium thiocyanate and 60 ml of dimethylformamide was stirred for 4 hours at 130°-140° C. The reaction solution was cooled to room temperature (hereinafter means "5°-20° C."), to which a mixture of 200 ml of diethyl ether and 200 ml of water was added. The ethereal layer was collected. The aqueous layer was extracted with 150 ml of diethyl ether. The combined ethereal layers were washed with a saturated saline, dried over anhydrous magnesium sulfate and distilled to remove the solvent. The residue was distilled under reduced pressure to obtain 12.4 g of 3-hydroxy-2,2-dimethyl-1-propylthiocyanate.

1. custom"5°-20° C."
2. additionwas added
3. customThe ethereal layer was collected
4. extractionThe aqueous layer was extracted with 150 ml of diethyl ether
5. washThe combined ethereal layers were washed with a saturated saline
6. dry with materialdried over anhydrous magnesium sulfate
7. distillationdistilled
8. customto remove the solvent
9. distillationThe residue was distilled under reduced pressure

ORDレコード

ord-02543adcd5c04215b3f3709bef51e2fd

出典データセット

uspto-grants-1992_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05155108