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

HRID 69490ノート

反応式

HRID 69490 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
130 °C

実験手順

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+).

後処理

  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)

出典と根拠

ORDレコード
ord-f1bdf2c6f30a4f709d03ca79a17f77db
出典データセット
uspto-grants-2014_09
特許番号
US08822495B2

反応ノート

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