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Hydrochloric Acid → N-(Phenylsulfonyl)-tetrahydro-2-nitromethylene-2H-1,3-thiazine

HRID 371347
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HRID 371347 반응식
CC(C)([O-])C.[K+].[SH:7][CH2:8][CH2:9][CH2:10][NH:11][S:12]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)(=[O:14])=[O:13].Cl[C:22](Cl)=[CH:23][N+:24]([O-:26])=[O:25].Cl.[Cl-].[Na+]>C(O)(C)(C)C>[C:15]1([S:12]([N:11]2[CH2:10][CH2:9][CH2:8][S:7][C:22]2=[CH:23][N+:24]([O-:26])=[O:25])(=[O:14])=[O:13])[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 5234Sodium ChlorideHCID 122195711,1-Dichloro-2-nitroetheneHCID 20238482N-(3-Mercaptopropyl)benzenesulfonamideHCID 23665647Potassium tert-butoxide

생성물 1

HCID 53713608N-(Phenylsulfonyl)-tetrahydro-2-nitromethylene-2H-1,3-thiazine

시약·촉매·용매 1

HCID 6386tert-Butanol용매

실험 절차

0.22 g of potassium t-butoxide was added drop-by-drop over 10 minutes to a solution of 0.23 g of 3 in 5 ml of t-butanol, under nitrogen. The resulting mixture was added drop-by-drop over 20 minutes to 0.30 g of 13A. After 20 minutes at room temperature, the mixture was poured into 2% hydrochloric acid saturated with sodium chloride, the resulting mixture was extracted with methylene chloride, the solvent was evaporated from the extract and the residue was purified over silica gel, using methylene chloride as eluent, to give 25, m.p: 106°-107° C.

후처리

  1. extractionthe resulting mixture was extracted with methylene chloride
  2. customthe solvent was evaporated from the
  3. extractionextract
  4. customthe residue was purified over silica gel

출처 및 근거

ORD 기록
ord-aa261ecb44a94b3ca6b1d920bea0bfc3
출처 데이터셋
uspto-grants-1985_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04531002

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