Cyanogen Chloride → 5-Chloro-1H-tetrazole-1-acetic acid ethyl ester

HRID 67701

反応式

HRID 67701 の反応式
[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]=1

参加物

4

反応物 2

HCID 10477Cyanogen ChlorideHCID 69480Acetic acid, azido-, ethyl ester

生成物 1

HCID 127857925-Chloro-1H-tetrazole-1-acetic acid ethyl ester収率 78%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  1. additionA mixture of 130 g
  2. temperatureAfter the reaction mixture had cooled
  3. filtrationthe solution was filtered
  4. customevaporated in vacuo
  5. customyielding a yellow crystalline mass of product
  6. customThe yellow crystals were recrystallized from aqueous ethyl alcohol
  7. customgave 149 g

出典と根拠

ORDレコード
ord-c63d467c6f9d4845a12de24553c24ec2
出典データセット
uspto-grants-1982_08
特許番号
US04346076

関連ノート

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