HCID 68158227、化合物 → 1392811-96-9
反応式
C[O:2][CH:3](OC)[C:4]1[C@H:8]2[CH2:9][O:10][CH2:11][C@H:7]2[O:6][N:5]=1>FC(F)(F)C(O)=O.O>[O:6]1[C@@H:7]2[CH2:11][O:10][CH2:9][C@@H:8]2[C:4]([CH:3]=[O:2])=[N:5]1参加物
4
実験手順
A solution of (3aS,6aS)-rel-3-dimethoxymethyl-3a,4,6,6a-tetrahydro-furo[3,4-d]isoxazole (35.3 mmol) in trifluoroacetic acid (30 ml) was treated with water (1.3 ml). The mixture was stirred at room temperature for 30 minutes. For the workup, the reaction mixture was diluted with water (100 ml) and extracted three times with dichloromethane. The combined organic layers were dried over sodium sulphate and evaporated. The crude product was purified by chromatography on silica gel using a 5:1-mixture of dichloromethane and heptane as the eluent. The (3aS,6aS)-rel-3a,4,6,6a-tetrahydro-furo[3,4-d]isoxazole-3-carbaldehyde (4.79 g, 96% yield) was obtained as a yellow oil. MS: m/z=144.0 [M+H]+.
後処理
- extractionextracted three times with dichloromethane
- dry with materialThe combined organic layers were dried over sodium sulphate
- customevaporated
- customThe crude product was purified by chromatography on silica gel using a 5
出典と根拠
- ORDレコード
- ord-437633aca92b49149d2b420fd225b27b
- 出典データセット
- uspto-grants-2013_03
- 特許番号
- US08404680B2
反応ノート
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