4H-1-Benzopyran-2-carboxylic acid, 4-oxo-, methyl ester → HCID 12536095, 화합물

HRID 574122노트

반응식

HRID 574122 반응식
[O:1]=[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[O:5][C:4]([C:12](OC)=[O:13])=[CH:3]1.[BH4-].[Na+]>CO>[OH:13][CH2:12][C:4]1[O:5][C:6]2[C:11]([C:2](=[O:1])[CH:3]=1)=[CH:10][CH:9]=[CH:8][CH:7]=2

참가 물질

4

반응물 2

HCID 290574H-1-Benzopyran-2-carboxylic acid, 4-oxo-, methyl esterHCID 4311764Sodium borohydride

생성물 1

HCID 12536095HCID 12536095, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

500 mg of methyl 4-oxo-4H-chromene-2-carboxylate were dissolved in 25 ml of anhydrous methanol at room temperature, and NaBH4 was thereafter added to the solution slowly, until the starting material was no longer detected by TLC (about 300 mg). The solvent was then evaporated and a mixture of 1.1 gram of NaH2PO4.2H2O in 30 ml of water was added to the resulting residue. The pH of the mixture was maintained between 5 and 9, so as to prevent decomposition of chromone. The aqueous solution was washed with chloroform (3×50 ml) and the combined organic extracts were dried over Na2SO4. The solvent was evaporated to give 2-(hydroxymethyl)-4H-chromen-4-one which was used without future purification.

후처리

  1. customThe solvent was then evaporated
  2. additiona mixture of 1.1 gram of NaH2PO4.2H2O in 30 ml of water
  3. additionwas added to the resulting residue
  4. temperatureThe pH of the mixture was maintained between 5 and 9
  5. washThe aqueous solution was washed with chloroform (3×50 ml)
  6. dry with materialthe combined organic extracts were dried over Na2SO4
  7. customThe solvent was evaporated

출처 및 근거

ORD 기록
ord-cfc367471d9e424f9b8be84b6d252a78
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09034872B2

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