Lithium azide → HCID 11994354, 화합물

HRID 1741482노트

반응식

HRID 1741482 반응식
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]

참가 물질

4

반응물 2

HCID 88163Lithium azideHCID 18660145HCID 18660145, 화합물

생성물 1

HCID 11994354HCID 11994354, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6cffc8195cad4dce86b7aee1ac91910d
출처 데이터셋
uspto-grants-1999_10
특허 번호
US05972984

반응 노트

불러오는 중…