Triethylamine → HCID 86604803, 화합물

HRID 856156노트

반응식

HRID 856156 반응식
[Cl:1][C:2]1[NH:3][CH:4]=[C:5]([N+:7]([O-:9])=[O:8])[N:6]=1.[N+:10]([C:13]1[CH:26]=[CH:25][C:16]([C:17]([O:19][CH2:20][C@:21]2([CH3:24])[CH2:23][O:22]2)=[O:18])=[CH:15][CH:14]=1)([O-:12])=[O:11].C(N(CC)CC)C>C(OCC)(=O)C>[Cl:1][C:2]1[N:3]([CH2:24][C@@:21]([OH:22])([CH3:23])[CH2:20][O:19][C:17](=[O:18])[C:16]2[CH:15]=[CH:14][C:13]([N+:10]([O-:12])=[O:11])=[CH:26][CH:25]=2)[CH:4]=[C:5]([N+:7]([O-:9])=[O:8])[N:6]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 147239Oxiranemethanol, 2-methyl-, 4-nitrobenzoate, (2S)-HCID 178526855HCID 178526855, 화합물

생성물 1

HCID 86604803HCID 86604803, 화합물수율 87.2%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
62.5 °C

실험 절차

2-Chloro-4-nitro-1H-imidazole (3 g, 20.34 mmol) and (S)-2-methyloxiran-2-ylmethyl 4-nitrobenzoate (5.31 g, 22.37 mmol) were dissolved in ethyl acetate (10 ml). Triethylamine (0.57 ml, 4.07 mmol) was added to the solution, and the resulting mixture was stirred at 60-65° C. for 10 hours. The reaction mixture was concentrated under reduced pressure. Ethyl acetate (3 ml) and toluene (30 ml) were added to the residue, and the resulting precipitates were filtered off to afford (S)-2-chloro-4-nitro-1-[2-hydroxy-3-(4-nitrobenzoyloxy)-2-methylpropyl]imidazole (6.82 g, yield 87%) as a yellow powder.

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. additionEthyl acetate (3 ml) and toluene (30 ml) were added to the residue
  3. customthe resulting precipitates
  4. filtrationwere filtered off

출처 및 근거

ORD 기록
ord-110b213b7e8f41b0b7b1b6666a146a53
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07262212B2

반응 노트

불러오는 중…