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Water → N-(2-(4-nitro-1H-pyrazol-1-yl)ethyl)methanesulfonamide

HRID 714903
ノート
印刷プレビュー

反応式

HRID 714903 の反応式
Cl.[N+:2]([C:5]1[CH:6]=[N:7][N:8]([CH2:10][CH2:11][NH2:12])[CH:9]=1)([O-:4])=[O:3].C(N(CC)CC)C.[CH3:20][S:21](Cl)(=[O:23])=[O:22].O>O1CCCC1>[N+:2]([C:5]1[CH:6]=[N:7][N:8]([CH2:10][CH2:11][NH:12][S:21]([CH3:20])(=[O:23])=[O:22])[CH:9]=1)([O-:4])=[O:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 717566062-(4-nitro-1H-pyrazol-1-yl)ethan-1-amine hydrochloride

生成物 1

HCID 117840477N-(2-(4-nitro-1H-pyrazol-1-yl)ethyl)methanesulfonamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 2-(4-nitro-1H-pyrazol-1-yl)ethanamine hydrochloride (1.0 g) obtained in Step B of Example 348 in tetrahydrofuran (30 mL) were added triethylamine (2.2 mL) and methanesulfonyl chloride (0.60 mL) in an ice bath, and the mixture was stirred at room temperature for 3 hr. To the reaction mixture was added water, and the mixture was extracted with ethyl acetate. The obtained organic layer was washed with water and saturated brine, and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was recrystallized (hexane/ethyl acetate) to give the title compound (880 mg).

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe obtained organic layer was washed with water and saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. customThe residue was recrystallized (hexane/ethyl acetate)

出典と根拠

ORDレコード
ord-d045afa469744c87b53664a457eac322
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09187453B2

反応ノート

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