Triethylamine → HCID 18961068, 화합물

HRID 1708197노트

반응식

HRID 1708197 반응식
C(N(CC)CC)C.C1(P(N=[N+]=[N-])(C2C=CC=CC=2)=O)C=CC=CC=1.[O:25]=[C:26]1[NH:30][CH2:29][CH:28]([C:31]([OH:33])=O)[S:27]1.[N+]([O-])(O)=O.[N+:38]([O:41][CH2:42][CH2:43][NH2:44])([O-:40])=[O:39]>O1CCCC1>[N+:38]([O:41][CH2:42][CH2:43][NH:44][C:31]([CH:28]1[S:27][C:26](=[O:25])[NH:30][CH2:29]1)=[O:33])([O-:40])=[O:39]

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 78397Ethanol, 2-amino-, 1-nitrate, nitrate (1:1)HCID 199401P,P-Diphenylphosphinic azideHCID 189610442-Oxo-1,3-thiazolidine-5-carboxylic acid

생성물 1

HCID 18961068HCID 18961068, 화합물수율 83.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

0.85 ml of triethylamine and 0.53 ml of diphenylphosphoryl azide were added, whilst ice-cooling, to a suspension of 0.30 g of 2-oxothiazolidine-5-carboxylic acid (prepared as described in Preparation 3) and 0.41 g of N-(2-nitrooxyethyl)amine nitrate in 10 ml of dry tetrahydrofuran, and the resulting mixture was stirred at room temperature for 2.5 hours. At the end of this time, the solvent was removed by distillation under reduced pressure, and the residue was purified by column chromatography through silica gel, using ethyl acetate as the eluent. The crude crystals thus obtained were triturated with diisopropyl ether, collected by filtration and washed to give 0.40 g of the title compound as a colorless powder, melting at 114°-115° C.

후처리

  1. customAt the end of this time, the solvent was removed by distillation under reduced pressure
  2. customthe residue was purified by column chromatography through silica gel
  3. customThe crude crystals thus obtained
  4. customwere triturated with diisopropyl ether
  5. filtrationcollected by filtration
  6. washwashed

출처 및 근거

ORD 기록
ord-fb900edafcfc4a1eb0f5a9553e55d211
출처 데이터셋
uspto-grants-1994_10
특허 번호
US05356918

반응 노트

불러오는 중…