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Pyrrolidine → 2-dimethoxymethyl-2-methyl-4-oxo-6-phenylsulfonyl-3,4-dihydro-2H-1-benzopyran

HRID 1463278
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HRID 1463278 반응식
[C:1]1([S:7]([C:10]2[CH:15]=[CH:14][C:13]([OH:16])=[C:12]([C:17](=[O:19])[CH3:18])[CH:11]=2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:20][C:21]([CH:23]([O:26][CH3:27])[O:24][CH3:25])=O.N1CCCC1>C1(C)C=CC=CC=1>[CH3:25][O:24][CH:23]([O:26][CH3:27])[C:21]1([CH3:20])[CH2:18][C:17](=[O:19])[C:12]2[CH:11]=[C:10]([S:7]([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)(=[O:9])=[O:8])[CH:15]=[CH:14][C:13]=2[O:16]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 31268PyrrolidineHCID 80650Pyruvic aldehyde dimethyl acetalHCID 189877381-(5-Benzenesulfonyl-2-hydroxy-phenyl)-ethanone

생성물 1

HCID 189877432-dimethoxymethyl-2-methyl-4-oxo-6-phenylsulfonyl-3,4-dihydro-2H-1-benzopyran

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

In 100 ml of toluene were dissolved 10 g of the compound obtained in step 4, 6.5 ml of pyruvic aldehyde dimethyl acetal and 1.5 ml of pyrrolidine. The resultant solution was heated to reflux for 16 hours and concentrated reduced pressure to obtain residue, which was purified by silica gel column chormatography using as an eluent a mixture of hexane and ethyl acetate (2:1) to obtain 11 g of the title compound.

후처리

  1. temperatureto reflux for 16 hours
  2. concentrationconcentrated reduced pressure
  3. customto obtain residue, which
  4. customwas purified by silica gel column chormatography
  5. additiona mixture of hexane and ethyl acetate (2:1)

출처 및 근거

ORD 기록
ord-38af4762e5104fb98719c0b01516ec91
출처 데이터셋
uspto-grants-1994_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05300511

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