1H-Benzotriazole, 1-hydroxy-, ammonium salt (1:1) → HCID 117840516, 화합물

HRID 714825노트

반응식

HRID 714825 반응식
[CH3:1][C:2]([N:7]1[CH:11]=[C:10]([N+:12]([O-:14])=[O:13])[CH:9]=[N:8]1)([CH3:6])[C:3](O)=[O:4].Cl.C([N:18]=C=NCCCN(C)C)C.N.ON1C2C=CC=CC=2N=N1.C(=O)([O-])O.[Na+]>CN(C)C=O>[CH3:1][C:2]([N:7]1[CH:11]=[C:10]([N+:12]([O-:14])=[O:13])[CH:9]=[N:8]1)([CH3:6])[C:3]([NH2:18])=[O:4]

참가 물질

6

반응물 4

HCID 1131751H-Benzotriazole, 1-hydroxy-, ammonium salt (1:1)HCID 516892Sodium BicarbonateHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 7017087α,α-Dimethyl-4-nitro-1H-pyrazole-1-acetic acid

생성물 1

HCID 117840516HCID 117840516, 화합물수율 83.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 2-methyl-2-(4-nitro-1H-pyrazol-1-yl)propanoic acid (1.2 g) obtained in Step A of Example 109 in N,N-dimethylformamide (10 mL) were added 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (1.3 g) and 1-hydroxybenzotriazole ammonia salt (1.4 g), and the mixture was stirred overnight at room temperature. To the reaction mixture was added saturated aqueous sodium hydrogen carbonate solution, and the mixture was extracted with ethyl acetate. The obtained organic layer was washed successively with water and saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (NH, ethyl acetate) to give the title compound (1.0 g).

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe obtained organic layer was washed successively with water and saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (NH, ethyl acetate)

출처 및 근거

ORD 기록
ord-9282b33823e94f81870ff8ea6015fa57
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09187453B2

반응 노트

불러오는 중…