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Hydrochloric Acid → 4-(Tert-butyl)-n-{3-(2-hydroxyethoxy)-1-methyl-4-[4-(trifluoromethyl)phenyl]-1h-pyrazol-5-yl}benzenesulfonamide

HRID 1368581
ノート
印刷プレビュー

反応式

HRID 1368581 の反応式
[C:1]([C:5]1[CH:10]=[CH:9][C:8]([S:11]([N:14]([C:21]2[N:25]([CH3:26])[N:24]=[C:23]([O:27][CH2:28][CH2:29][OH:30])[C:22]=2[C:31]2[CH:36]=[CH:35][C:34]([C:37]([F:40])([F:39])[F:38])=[CH:33][CH:32]=2)COCCOC)(=[O:13])=[O:12])=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].Cl>C(O)C>[C:1]([C:5]1[CH:6]=[CH:7][C:8]([S:11]([NH:14][C:21]2[N:25]([CH3:26])[N:24]=[C:23]([O:27][CH2:28][CH2:29][OH:30])[C:22]=2[C:31]2[CH:32]=[CH:33][C:34]([C:37]([F:40])([F:38])[F:39])=[CH:35][CH:36]=2)(=[O:12])=[O:13])=[CH:9][CH:10]=1)([CH3:4])([CH3:2])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 222819664-(tert-butyl)-N-{3-(2-hydroxyethoxy)-1-methyl-4-[4-(trifluoromethyl)phenyl]-1H-pyrazol-5-yl}-N-[(2-methoxyethoxy)methyl]benzenesulfonamide

生成物 1

HCID 222819594-(Tert-butyl)-n-{3-(2-hydroxyethoxy)-1-methyl-4-[4-(trifluoromethyl)phenyl]-1h-pyrazol-5-yl}benzenesulfonamide

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To 4-(tert-butyl)-N-{3-(2-hydroxyethoxy)-1-methyl-4-[4-(trifluoromethyl)phenyl]-1H-pyrazol-5-yl}-N-[(2-methoxyethoxy)methyl]benzenesulfonamide (Preparation 12) in ethanol (1.5 ml) was added hydrochloric acid (6M, 1.5 ml). The reaction mixture was refluxed for 5 hours and then left at room temperature overnight. The reaction was concentrated under reduced pressure and the residue was partitioned between water (10 ml) and ethyl acetate (10 ml). The aqueous was extracted with ethyl acetate (2×20 ml). The organics were combined, dried over magnesium sulfate, filtered and concentrated under reduced pressure to yield the desired product (120 mg) as a white solid. Taken on crude to the next step.

後処理

  1. temperatureThe reaction mixture was refluxed for 5 hours
  2. concentrationThe reaction was concentrated under reduced pressure
  3. customthe residue was partitioned between water (10 ml) and ethyl acetate (10 ml)
  4. extractionThe aqueous was extracted with ethyl acetate (2×20 ml)
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-0463e8a1c79f46d985e5e92f639a0821
出典データセット
uspto-grants-2003_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06573270B1

反応ノート

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