1H-Benzotriazole, 1-hydroxy-, ammonium salt (1:1) → HCID 117840516、化合物

HRID 714825ノート

反応式

HRID 714825 の反応式
[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]

参加物

6

反応物 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

生成物 1

HCID 117840516HCID 117840516、化合物収率 83.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-9282b33823e94f81870ff8ea6015fa57
出典データセット
uspto-grants-2015_11
特許番号
US09187453B2

反応ノート

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