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Dichloromethane → HCID 13852481, 화합물

HRID 622058
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HRID 622058 반응식
[NH2:1][S:2]([C:5]1[CH:16]=[CH:15][CH:14]=[CH:13][C:6]=1[C:7]([O:9][CH2:10][CH2:11][OH:12])=[O:8])(=[O:4])=[O:3].C(Cl)Cl.[CH3:20][Si:21](Cl)([CH3:23])[CH3:22]>C(N(CC)CC)C>[NH2:1][S:2]([C:5]1[CH:16]=[CH:15][CH:14]=[CH:13][C:6]=1[C:7]([O:9][CH2:10][CH2:11][O:12][Si:21]([CH3:23])([CH3:22])[CH3:20])=[O:8])(=[O:3])=[O:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 6397ChlorotrimethylsilaneHCID 138524802-Hydroxyethyl 2-sulfamoylbenzoate

생성물 1

HCID 13852481HCID 13852481, 화합물

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

To a slurry of 12.25 g of 2-aminosulfonylbenzoic acid, 2-hydroxyethyl ester, 125 ml of dry methylene chloride, and 7.7 ml of triethylamine was added dropwise over 10 minutes 6.3 ml of trimethylsilyl chloride (exotherm to 36° C.). The resulting solution was allowed to stand at ambient temperature for 18 hours and then washed with saturated sodium chloride solution, dried (MgSO4), and the solvent removed under reduced pressure to give an oil which was chromatographed on silica gel eluting with 25% EtOAc:hexane to give a colorless oil which slowly crystallized. Trituration with hexane gave 8.0 g of white crystals, m.p. 72°-76° C.

후처리

  1. washwashed with saturated sodium chloride solution
  2. dry with materialdried (MgSO4)
  3. customthe solvent removed under reduced pressure
  4. customto give an oil which
  5. customwas chromatographed on silica gel eluting with 25% EtOAc
  6. customhexane to give a colorless oil which
  7. customslowly crystallized

출처 및 근거

ORD 기록
ord-73f5bab4a9d04ee8bcd8b3d011bbca23
출처 데이터셋
uspto-grants-1988_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04769060

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