Ammonia → HCID 178514025、化合物

HRID 2049560ノート

反応式

HRID 2049560 の反応式
[SH:1][C:2]1(CC(OCC)=O)[NH:6][NH:5][N:4]=[N:3]1.[NH3:13].[CH2:14]([OH:16])[CH3:15]>>[SH:1][C:2]1[N:3]([CH2:15][C:14]([NH2:13])=[O:16])[N:4]=[N:5][N:6]=1

参加物

4

反応物 3

HCID 222AmmoniaHCID 702EthanolHCID 86736933Ethyl 5-mercapto-1H-tetrazol-5-ylacetate

生成物 1

HCID 178514025HCID 178514025、化合物

実験手順

Ethyl 5-mercapto-1H-tetrazol-5-ylacetate (15.0 g) was dissolved in ethanol (50 ml), the solution was saturated with ammonia gas then set aside for 36 hours. The precipitated mass was collected, washed with ethanol (20 ml), dried and dissolved in water (100 ml). The solution was treated with decolourising charcoal, filtered, acidified with concentrated hydrochloric acid and cooled in an ice bath. The product crystallised as needles and was collected, washed with a little water and dried in vacuo, 9.51 g., (75.0%) m.p. 214°-216° C. (d), νmax (nujol) 1695 cm-1 ; δ[(CD3)2SO], 7.72 (2H,d, J=22 Hz, --NH2), 5.02 (2H,s, --CH2 --). Found: C, 22.39; H, 2.18; N, 43.82; S, 20.16. C3H5N5OS requires: C, 22.64; H, 3.17; N, 44.00; S, 20.14%.

後処理

  1. customThe precipitated mass was collected
  2. washwashed with ethanol (20 ml)
  3. customdried
  4. dissolutiondissolved in water (100 ml)
  5. additionThe solution was treated with decolourising charcoal
  6. filtrationfiltered
  7. temperaturecooled in an ice bath
  8. customThe product crystallised as needles
  9. customwas collected
  10. washwashed with a little water
  11. customdried in vacuo, 9.51 g

出典と根拠

ORDレコード
ord-6e3dfbd7871d4266b38c56a7aac12775
出典データセット
uspto-grants-1980_04
特許番号
US04198406

反応ノート

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