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Ethyl bromoacetate → HCID 13922855, 화합물

HRID 2232343
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HRID 2232343 반응식
Br[CH2:2][C:3]([O:5][CH2:6][CH3:7])=[O:4].[OH:8][C:9]1[CH:10]=[CH:11][C:12]2[CH:16]=[C:15]([S:17](=[O:20])(=[O:19])[NH2:18])[S:14][C:13]=2[CH:21]=1.C(=O)(O)[O-].[K+].C(=O)([O-])[O-].[K+].[K+]>CS(C)=O.O>[CH2:6]([O:5][C:3]([CH2:2][O:8][C:9]1[CH:10]=[CH:11][C:12]2[CH:16]=[C:15]([S:17](=[O:19])(=[O:20])[NH2:18])[S:14][C:13]=2[CH:21]=1)=[O:4])[CH3:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 7748Ethyl bromoacetateHCID 11430Potassium CarbonateHCID 146921L 650719HCID 516893Potassium Bicarbonate

생성물 1

HCID 13922855HCID 13922855, 화합물수율 38.1%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매
HCID 962
Water
용매
2회

실험 절차

To a solution of ethyl bromoacetate (1.2 ml, 11 mmol) and 6-hydroxy-2-sulfamoylbenzo[b]thiophene (2.29 g, 10 mmol) in DMSO (10 ml) was added dropwise a solution of potassium bicarbonate (1.0 g, 10 mmol) and potassium carbonate (0.13 g, 1 mmol) in water (7 ml). The mixture was stirred for 1-2 days, then diluted with water. The precipitated product was collected dissolved in ethyl acetate, dried (Na2SO4) and evaporated to dryness. The residue was recrystallized from hot ethyl acetate, boiling off solvent until crystallization began, to give 1.2 g of product, m.p. 182°-184° C.

후처리

  1. customThe precipitated product was collected
  2. dissolutiondissolved in ethyl acetate
  3. dry with materialdried (Na2SO4)
  4. customevaporated to dryness
  5. customThe residue was recrystallized from hot ethyl acetate
  6. customuntil crystallization

출처 및 근거

ORD 기록
ord-98d9c8995cb249779d2735aba4775672
출처 데이터셋
uspto-grants-1988_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04788192

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