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Water → 4-(1,1-dioxoisothiazolidin-2-yl)-6-mesyl-2,2-dimethyl-2H-1-benzopyran

HRID 1030215
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HRID 1030215 반응식
O[C@H:2]1[C@H:7]([N:8]2[CH2:12][CH2:11][CH2:10][S:9]2(=[O:14])=[O:13])[C:6]2[CH:15]=[C:16]([S:19]([CH3:22])(=[O:21])=[O:20])[CH:17]=[CH:18][C:5]=2[O:4][C:3]1([CH3:24])[CH3:23].C(OC(=O)C)(=O)C.O>N1C=CC=CC=1>[O:14]=[S:9]1(=[O:13])[CH2:10][CH2:11][CH2:12][N:8]1[C:7]1[C:6]2[CH:15]=[C:16]([S:19]([CH3:22])(=[O:20])=[O:21])[CH:17]=[CH:18][C:5]=2[O:4][C:3]([CH3:23])([CH3:24])[CH:2]=1
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참가 물질

5

반응물 3

HCID 962WaterHCID 7918Acetic AnhydrideHCID 67792343trans-3,4-dihydro-3-hydroxy-4-(1,1-dioxoisothiazolidin-2-yl)-6-mesyl-2,2-dimethyl-2H-1-benzopyran

생성물 1

HCID 157348204-(1,1-dioxoisothiazolidin-2-yl)-6-mesyl-2,2-dimethyl-2H-1-benzopyran수율 46%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A solution of trans-3,4-dihydro-3-hydroxy-4-(1,1-dioxoisothiazolidin-2-yl)-6-mesyl-2,2-dimethyl-2H-1-benzopyran (0.32 g) in pyridine (10 ml) was treated with acetic anhydride (5 ml), and the mixture was stood at room temperature overnight. The reaction mixture was poured into water and extracted with ethyl acetate. The extract was washed successively with 1N hydrochloric acid, a saturated aqueous solution of sodium bicarbonate and brine, and then dried over anhydrous magnesium sulfate. Removal of the solvent under reduced pressure gave the crude product, which was purified by recrystallization from ethyl acetate to give 4-(1,1-dioxoisothiazolidin-2-yl)-6-mesyl-2,2-dimethyl-2H-1-benzopyran (0.14 g).

후처리

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed successively with 1N hydrochloric acid
  3. dry with materiala saturated aqueous solution of sodium bicarbonate and brine, and then dried over anhydrous magnesium sulfate
  4. customRemoval of the solvent under reduced pressure
  5. customgave the crude product, which
  6. customwas purified by recrystallization from ethyl acetate

출처 및 근거

ORD 기록
ord-12da0770602f48eab66cac55d9960738
출처 데이터셋
uspto-grants-1992_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05104890

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