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

HRID 1030215
ノート
印刷プレビュー

反応式

HRID 1030215 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-12da0770602f48eab66cac55d9960738
出典データセット
uspto-grants-1992_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05104890

反応ノート

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