Cyanogen Chloride → 5-Chloro-1H-tetrazole-1-acetic acid ethyl ester
반응식
[N:1]([CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6])=[N+:2]=[N-:3].[N:10]#[C:11][Cl:12]>C(OCC)(=O)C>[Cl:12][C:11]1[N:1]([CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6])[N:2]=[N:3][N:10]=1참가 물질
4
실험 절차
A mixture of 130 g. (1 mole) of ethyl azidoacetate prepared as described in part A and 96 g. (1.56 mole) of cyanogen chloride was heated at a temperature of 125° C. for 20 hours. After the reaction mixture had cooled, the reaction product mixture was dissolved in ethyl acetate, and the solution was filtered and evaporated in vacuo yielding a yellow crystalline mass of product. The yellow crystals were recrystallized from aqueous ethyl alcohol and gave 149 g. (78% yield) of ethyl 5-chloro-1H-tetrazol-1-ylacetate as pale yellow crystals melting at about 57°-60° C.
후처리
- additionA mixture of 130 g
- temperatureAfter the reaction mixture had cooled
- filtrationthe solution was filtered
- customevaporated in vacuo
- customyielding a yellow crystalline mass of product
- customThe yellow crystals were recrystallized from aqueous ethyl alcohol
- customgave 149 g
출처 및 근거
- ORD 기록
- ord-c63d467c6f9d4845a12de24553c24ec2
- 출처 데이터셋
- uspto-grants-1982_08
- 특허 번호
- US04346076
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