2-Chloroethyl isocyanate → (2-Chloroethyl)carbamyl azide
반응식
[Cl:1][CH2:2][CH2:3][N:4]=[C:5]=[O:6].[N-:7]=[N+:8]=[N-:9].[Na+]>C1C=CC=CC=1.Cl>[Cl:1][CH2:2][CH2:3][NH:4][C:5]([N:7]=[N+:8]=[N-:9])=[O:6]참가 물질
5
반응 조건
- 온도
- 0 °C
실험 절차
A solution of 2-chloroethyl isocyanate (0.2 mole) in 100 ml of benzene was slowly added to a stirred solution of activated sodium azide (0.2 mole) in 100 ml of hydrochloric acid (13%) maintained at 0° C. The two-phase reaction mixture was stirred for 4 hours at 0° C. and the water phase was removed. 2-chloroethylcarbamoyl azide was crystallized from benzene/petroleum ether in the form of white needles. Yield: 88%. M.P. 49.6 to 50.2° C. NMR(CDCl3 -TMS)δ=3.4 to 3.9 ppm (unres., 4H, CH2 --CH2Cl); 6.12 ppm (br, s, iH, NH); MS(14 v):m/e 148(M+), m/e 106(M--N3)+, m/e 105 (M--HN3)+=base peak. An intensity ratio of m/e 148 / m/e 150 is typical for a monochlorinated compound.
후처리
- customThe two-phase reaction mixture
- customthe water phase was removed
- custom2-chloroethylcarbamoyl azide was crystallized from benzene/petroleum ether in the form of white needles
출처 및 근거
- ORD 기록
- ord-a0178d1904114babb7649513b46595b2
- 출처 데이터셋
- uspto-grants-1979_04
- 특허 번호
- US04150146
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