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Water → 3-Amino-6-chloro-2-hydroxy-N-methoxy-N-ethyl-benzenesulfonamide

HRID 1669615
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HRID 1669615 반응식
[CH2:1]([N:3]([O:21][CH3:22])[S:4]([C:7]1[C:15]2[O:14]C(C(C)(C)C)=[N:12][C:11]=2[CH:10]=[CH:9][C:8]=1[Cl:20])(=[O:6])=[O:5])[CH3:2].S(=O)(=O)(O)O.O>O1CCOCC1>[NH2:12][C:11]1[C:15]([OH:14])=[C:7]([S:4]([N:3]([O:21][CH3:22])[CH2:1][CH3:2])(=[O:6])=[O:5])[C:8]([Cl:20])=[CH:9][CH:10]=1
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참가 물질

5

반응물 3

HCID 962WaterHCID 1118Sulfuric AcidHCID 866386352-tert-Butyl-6-chloro-benzooxazole-7-sulfonic acid ethyl-methoxy-amide

생성물 1

HCID 866386363-Amino-6-chloro-2-hydroxy-N-methoxy-N-ethyl-benzenesulfonamide

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
80 °C

실험 절차

2-tert-Butyl-6-chloro-benzooxazole-7-sulfonic acid ethyl-methoxy-amide (2.7 g, 7.78 mmol) in dioxane (15 ml) was treated with a mixture of concentrated sulphuric acid (3.5 ml) and water (3.5 ml). The reaction mixture was heated at 80° C. for a total of 8 h and then allowed to cool to RT. Dioxane was removed in vacuo and the resulting aqueous mixture was treated with 1M NaOH (aq) until pH7 was attained. The reaction mixture was extracted with EtOAc, dried (MgSO4) and concentrated in vacuo to afford the title compound as a brown solid; [M+H]+ 281.1.

후처리

  1. temperatureto cool to RT
  2. customDioxane was removed in vacuo
  3. additionthe resulting aqueous mixture was treated with 1M NaOH (aq) until pH7
  4. extractionThe reaction mixture was extracted with EtOAc
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-115d1e8dfb994829a1663d5aa53af45e
출처 데이터셋
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07989497B2

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