Iodine → Benzene, (diazomethyl)-

To benzaldehyde hydrazone (5.95 g, 0.05 moles) in 1,2-dichloroethane (50 ml) containing 1,1,3,3-tetramethylguanidine (26.4 ml) and iodine (2 ml, 1% w/v solution) was added peracetic acid solution (11.4 ml, 1.27 × 0.05 moles) over 12 minutes at 0°. The red solution, which was gently evolving nitrogen, was stirred for 20 minutes at 0° to -5° before being washed with water (5 × 250 ml) and made up to 250 ml in a volumetric flask. An aliquot (50 ml) treated with excess acetic acid yielded 199 ml gas at NTP which corresponded to a yield of diazoalkane of 88.9%.

1. washbefore being washed with water (5 × 250 ml)
2. custommade up to 250 ml in a volumetric flask
3. additionAn aliquot (50 ml) treated with excess acetic acid

ORDレコード

ord-76870d5574c74ff6bf704d4e8a40f82b

出典データセット

uspto-grants-1978_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04083837