Methanol → Methyl 1-(mercaptomethyl)cyclopropaneacetate
反応式
C([S:4][CH2:5][C:6]1([CH2:9][C:10]#N)[CH2:8][CH2:7]1)(=O)C.[OH2:12].OS(O)(=O)=O.[CH3:18][OH:19]>>[SH:4][CH2:5][C:6]1([CH2:9][C:10]([O:19][CH3:18])=[O:12])[CH2:7][CH2:8]1参加物
5
反応条件
- 温度
- 25 °C
実験手順
To a solution of the nitrile of Step 8 (45 g, 266 mmol) in MeOH (1.36 L) was added H2O(84 mL) and conc. H2SO4 (168 mL). The mixture was heated to reflux for 20 hr, cooled to 25° C., H2O(1 L) was added and the product was extracted with CH2Cl2 (2×1.5 L). The organic extract was washed with H2O and dried over Na2SO4. Concentration of the organic solution gave 36 g (93%) of the title compound.
後処理
- temperatureThe mixture was heated
- temperatureto reflux for 20 hr
- extractionthe product was extracted with CH2Cl2 (2×1.5 L)
- extractionThe organic extract
- washwas washed with H2O
- dry with materialdried over Na2SO4
出典と根拠
- ORDレコード
- ord-3561463f2f1f44499b54b2448ade42d8
- 出典データセット
- uspto-grants-1995_12
- 特許番号
- US05472964
反応ノート
読み込み中…