Hydrochloric Acid → 4-Hydrazinyl-1-methylpiperidine

温度

60 °C

A solution of 1 M borane in THF (30 mL) was added to solid 2.80 g (12.3 mmol) of tert-butyl N′-(1-Methyl-piperidin-4-ylidene)-hydrazinecarboxylate. The mixture was stirred under N2 for 16 h when 40 mL of 6M HCl was carefully added. The mixture was heated to 60° C. for 30 min. The mixture was concentrated in vacuo at ambient temperature for 2 days. Petroleum ether (200 mL) and powdered NaOH (5 g) were added, and the mixture was stirred manually for 30 min. The mixture was dried with MgSO4, filtered, and carefully concentrated to give 1.3 g of (1-methyl-piperidin-4-yl)-hydrazine.

1. additionwas carefully added
2. concentrationThe mixture was concentrated in vacuo at ambient temperature for 2 days
3. additionPetroleum ether (200 mL) and powdered NaOH (5 g) were added
4. dry with materialThe mixture was dried with MgSO4
5. filtrationfiltered
6. concentrationcarefully concentrated

ORDレコード

ord-7b6ff192016d496fbf220b53c76b1f33

出典データセット

uspto-grants-2009_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07514458B2