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Hydrochloric Acid → HCID 14404106, 화합물

HRID 465502
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HRID 465502 반응식
[C:1]([C:4]1[CH:9]=[CH:8][C:7]([S:10]([CH2:13][N+:14]([O-:16])=[O:15])(=[O:12])=[O:11])=[CH:6][CH:5]=1)(O)=[O:2].Cl>O1CCCC1>[OH:2][CH2:1][C:4]1[CH:9]=[CH:8][C:7]([S:10]([CH2:13][N+:14]([O-:16])=[O:15])(=[O:12])=[O:11])=[CH:6][CH:5]=1
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 14404103HCID 14404103, 화합물

생성물 1

HCID 14404106HCID 14404106, 화합물수율 25.9%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Borane-methyl sulphide complex (0.1 ml, 1 mmol) was added to a solution of (4-carboxyphenylsulphonyl)nitromethane (0.25 g, 1 mmol) in anhydrous tetrahydrofuran (5 ml) and the mixture was stirred for 2 hours. The mixture was acidified with 2M hydrochloric acid to pH 1 and extracted with ethyl acetate. The combined extracts were dried (MgSO4) and the solvent was removed by evaporation. The residue was purified by MPLC eluting with methanol/dichloromethane (1:50 v/v) to give (4-hydroxymethylphenylsulphonyl)nitromethane (0.06 g) m.p. 73°-75° C.; microanalysis, found: C, 41.6; H, 3.9; N, 5.8%; C8H9NO5S requires: C, 41.6; H, 3.9; N, 6.1%.

후처리

  1. extractionextracted with ethyl acetate
  2. dry with materialThe combined extracts were dried (MgSO4)
  3. customthe solvent was removed by evaporation
  4. customThe residue was purified by MPLC
  5. washeluting with methanol/dichloromethane (1:50 v/v)

출처 및 근거

ORD 기록
ord-75c3d65d7394459681bc7d10f53e5b14
출처 데이터셋
uspto-grants-1992_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05153227

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