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Water → 2-methyl-2-(4-nitro-1H-pyrazol-1-yl)propyl methanesulfonate

HRID 714831
ノート
印刷プレビュー

反応式

HRID 714831 の反応式
[CH3:1][C:2]([N:6]1[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[CH:8]=[N:7]1)([CH3:5])[CH2:3][OH:4].C(N(CC)CC)C.[CH3:21][S:22](Cl)(=[O:24])=[O:23].O>O1CCCC1>[CH3:21][S:22]([O:4][CH2:3][C:2]([CH3:1])([N:6]1[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[CH:8]=[N:7]1)[CH3:5])(=[O:24])=[O:23]
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 1178409402-Methyl-2-(4-nitro-pyrazol-1-yl)-propan-1-ol

生成物 1

HCID 1178409212-methyl-2-(4-nitro-1H-pyrazol-1-yl)propyl methanesulfonate

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 2-methyl-2-(4-nitro-1H-pyrazol-1-yl)propan-1-ol (13 g) obtained in Step G of Example 103 in tetrahydrofuran (100 mL) were added successively dropwise triethylamine (12 mL) and methanesulfonyl chloride (6.3 mL) at 0° C. under nitrogen atmosphere, and the mixture was stirred at room temperature for 2 hr. To the reaction mixture was added water, and the mixture was extracted with ethyl acetate. The obtained organic layer was washed with saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure to give the crude title compound (18 g).

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe obtained organic layer was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customthe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-9b95c9f84a2a415a95425145cf7c46d1
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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このページの内容参加物実験手順後処理出典と根拠反応ノート