Water → Ethyl 2-(hydroxymethyl)cyclopropanecarboxylate

温度

0 °C

Ethyl 2-formyl-1-cyclopropanecarboxylate (2 ml, 15.11 mmol) was dissolved in methanol (35 ml) and cooled to 0° C. under N2. Sodium borohydride (1.2 g, 31.7 mmol) was added in portions and resulting solution stirred at 0° C. for 2 h. The solution was then diluted by the dropwise addition of water, followed by the addition of EtOAc (100 mL). The aqueous layer was separated and extracted with EtOAc (2×50 mL). The combined organic layers were washed with brine, dried over sodium sulphate and concentrated in vacuo to give the title compound. TLC: 20% EtOAc/hexanes, high Rf: 0.35, low Rf: 0.3.

1. customresulting solution
2. customThe aqueous layer was separated
3. extractionextracted with EtOAc (2×50 mL)
4. washThe combined organic layers were washed with brine
5. dry with materialdried over sodium sulphate
6. concentrationconcentrated in vacuo

ORDレコード

ord-b04b0085714747b3a4f223f0a0842e48

出典データセット

uspto-grants-2014_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08895596B2