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

HRID 714831
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HRID 714831 반응식
[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]
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참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 1178409402-Methyl-2-(4-nitro-pyrazol-1-yl)-propan-1-ol

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-9b95c9f84a2a415a95425145cf7c46d1
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09187453B2

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