3,3-Bis(hydroxymethyl)-2,3-dihydro-4H-1-benzothiopyran-4-one → HCID 59756936, 화합물

HRID 1009213노트

반응식

HRID 1009213 반응식
[OH:1][CH2:2][C:3]1([CH2:14][OH:15])[C:12](=[O:13])[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[S:5][CH2:4]1.I([O-])(=O)(=O)=[O:17].[Na+]>CO.O>[OH:15][CH2:14][C:3]1([CH2:2][OH:1])[C:12](=[O:13])[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[S:5](=[O:17])[CH2:4]1

참가 물질

5

반응물 2

HCID 27640233,3-Bis(hydroxymethyl)-2,3-dihydro-4H-1-benzothiopyran-4-oneHCID 23667635Sodium periodate

생성물 1

HCID 59756936HCID 59756936, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매2회

실험 절차

A solution of 3,3-bis(hydroxymethyl)thiochroman-4-one (200 mg, 0.9 mmol) in MeOH (5 ml) was admixed with a solution of sodium metaperiodate (206 mg, 0.96 mmol) in water (2 ml) and stirred at RT for 72 h. The reaction mixture was diluted with water (10 ml) and extracted with EtOAc (3×30 ml), the combined organic phases were dried over sodium sulfate and the solvent was removed under reduced pressure. After column chromatography purification of the residue (silica gel, EtOAc), the desired product was obtained as a white solid (113 mg, 52% of theory, m.p. 108-111° C.).

후처리

  1. extractionextracted with EtOAc (3×30 ml)
  2. dry with materialthe combined organic phases were dried over sodium sulfate
  3. customthe solvent was removed under reduced pressure
  4. customAfter column chromatography purification of the residue (silica gel, EtOAc)

출처 및 근거

ORD 기록
ord-42f50f003db94066851b14c10cd962e1
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07973072B2

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