Sodium Azide → Butane, 3-azido-1,1,1-trifluoro-

1,1,1-Trifluoro-3-iodobutane (20.00 g, 0.084 mol) was added slowly to a stirred solution of sodium azide (13.00 g, 0.200 mol) in aqueous ethanol (60% ethanol, 200 ml) contained in a 500 ml flask (3-necked) with an argon lute, then refluxed for 11 h. The solution was extracted with ether (250 ml), which was washed and dried, and shown by g.l.c. analysis (2 m D.N.P. at 60°) to contain one major product, 3-azido-1,1,1-trifluorobutane, [approximately 9 g (estimated from g.l.c. analysis), 0.059 mol, 70%] which was not isolated because of the explosive hazard.

1. customcontained in a 500 ml flask
2. temperature(3-necked) with an argon lute, then refluxed for 11 h
3. extractionThe solution was extracted with ether (250 ml), which
4. washwas washed
5. customdried
6. customanalysis (2 m D.N.P. at 60°)
7. customwas not isolated because of the explosive hazard

ORDレコード

ord-6c7c5208a4184fbd9b9716f878f2b08e

出典データセット

uspto-grants-1985_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04524152