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2-Chloroethanol → 2-chloroethoxy-2-methyl-2H-indazole-3-sulfonamide

HRID 1378931
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HRID 1378931 반응식
CCOC(/N=N/C(OCC)=O)=O.[OH:13][C:14]1[C:15]2[C:19]([CH:20]=[CH:21][CH:22]=1)=[N:18][N:17]([CH3:23])[C:16]=2[S:24]([NH2:27])(=[O:26])=[O:25].[Cl:28][CH2:29][CH2:30]O.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C1COCC1.O>[Cl:28][CH2:29][CH2:30][O:13][C:14]1[C:15]2[C:19]([CH:20]=[CH:21][CH:22]=1)=[N:18][N:17]([CH3:23])[C:16]=2[S:24]([NH2:27])(=[O:26])=[O:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 342-ChloroethanolHCID 11776TriphenylphosphineHCID 5462977Diethyl azodicarboxylateHCID 135829371HCID 135829371, 화합물

생성물 1

HCID 867496182-chloroethoxy-2-methyl-2H-indazole-3-sulfonamide수율 26%

시약·촉매·용매 2

HCID 962Water
용매
HCID 8028Tetrahydrofuran용매

실험 절차

3.8 g (22 mmol) of diethylazo dicarboxylate was added to a solution containing 5 g (22 mmol) of 4-hydroxy-2-methyl-2H-indazole-3-sulfonamide, 1.8 g (22 mmol) of 2-chloroethanol and 5.8 g (22 mmol) of triphenylphosphine in 50 ml of THF, and the mixture was stirred at room temperature for 20 hours. The mixture was poured into water and extracted with ethyl acetate. The organic layer was washed with water, then concentrated and purified by column chromatography (hexane/ethyl acetate=2/1) to obtain 1.66 g (yield: 26%) of the desired product. Melting point: 177°-179° C.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with water
  3. concentrationconcentrated
  4. custompurified by column chromatography (hexane/ethyl acetate=2/1)

출처 및 근거

ORD 기록
ord-ee91f44886684ab694d18aa5ab51fbbe
출처 데이터셋
uspto-grants-1997_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05670452

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