Dimethylformamide → 6-((S)-2-Hydroxybutoxy)isochromen-1-one

HRID 69490노트

반응식

HRID 69490 반응식
[OH:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[C:8](=[O:12])[O:7][CH:6]=[CH:5]2.[O:13]1[C@@H:15]([CH2:16][CH3:17])[CH2:14]1.[F-].[Cs+].CN(C=O)C>O>[OH:13][C@@H:15]([CH2:16][CH3:17])[CH2:14][O:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[C:8](=[O:12])[O:7][CH:6]=[CH:5]2

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 25953Cesium fluorideHCID 10898629(2S)-2-EthyloxiraneHCID 668796996-Hydroxyisochromen-1-one

생성물 1

HCID 668791856-((S)-2-Hydroxybutoxy)isochromen-1-one

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
130 °C

실험 절차

A mixture of 6-Hydroxy-isochromen-1-one (405 mg), (S)-(−)-1,2-epoxybutane (361 mg), cesium fluoride (1.1 g) and DMF (5 mL) was stirred for 4 h at 130° C. After adding water it was extracted with dichloromethane, dried over magnesium sulfate and concentrated. The residue was purified by preparative HPLC. In this way the product was obtained with molecular weight 234.25 (C13H1404); MS (ESI): 235 (M+H+).

후처리

  1. extractionwas extracted with dichloromethane
  2. dry with materialdried over magnesium sulfate
  3. concentrationconcentrated
  4. customThe residue was purified by preparative HPLC
  5. customIn this way the product was obtained with molecular weight 234.25 (C13H1404)

출처 및 근거

ORD 기록
ord-f1bdf2c6f30a4f709d03ca79a17f77db
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822495B2

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