Lithium azide → HCID 11994354、化合物

HRID 1741482ノート

反応式

HRID 1741482 の反応式
CS(O[CH2:6][C@@H:7]1[CH2:11][CH2:10][CH2:9][N:8]1C(=O)C(F)(F)F)(=O)=O.[N-:18]=[N+:19]=[N-:20].[Li+]>CN(C=O)C>[N:18]([CH2:6][C@@H:7]1[CH2:11][CH2:10][CH2:9][NH:8]1)=[N+:19]=[N-:20]

参加物

4

反応物 2

HCID 88163Lithium azideHCID 18660145HCID 18660145、化合物

生成物 1

HCID 11994354HCID 11994354、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

In a flask protected by a safety screen, a solution of the product of step B (12.27 g, 0.042 mmol) and lithium azide (2.47 g, 0.051 mmol) in DMF (30 ml) was stirred at 45° C. for 18 hr. The solvent was evaporated in vacuo and the residue triturated with EtOAc (100 ml) and filtered. The filtrate was evaporated in vacuo and the residue dissolved in MeOH (255 ml) which was saturated with gaseous ammonia at 0° C. and then stirred at room temperature for 72 hr. The solvent was removed by distillation in vacuo to afford the title compound as an oil.

後処理

  1. customIn a flask protected by a safety screen
  2. customThe solvent was evaporated in vacuo
  3. customthe residue triturated with EtOAc (100 ml)
  4. filtrationfiltered
  5. customThe filtrate was evaporated in vacuo
  6. dissolutionthe residue dissolved in MeOH (255 ml) which
  7. customwas saturated with gaseous ammonia at 0° C.
  8. customThe solvent was removed by distillation in vacuo

出典と根拠

ORDレコード
ord-6cffc8195cad4dce86b7aee1ac91910d
出典データセット
uspto-grants-1999_10
特許番号
US05972984

反応ノート

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