Water → HCID 10909824、化合物
反応式
C([O:3][C:4]([C:6]1[S:10][CH:9]=[N:8][C:7]=1[CH:11]([CH3:13])[CH3:12])=O)C.CC(C[AlH]CC(C)C)C.O>C1(C)C=CC=CC=1>[OH:3][CH2:4][C:6]1[S:10][CH:9]=[N:8][C:7]=1[CH:11]([CH3:13])[CH3:12]参加物
5
実験手順
A solution of 5.9 g (30 mmol) of 4-isopropyl-thiazole-5-carboxylic acid ethyl ester (J. Chem. Soc., Perkin Trans. 1, 1982:159-164) in toluene (100 mL) was cooled in an ice bath under nitrogen and treated dropwise with DIBAL (150 mL of 1.0 M; 150 mmol). The mixture was stirred at low temperature for 45 minutes and then allowed to warm to room temperature overnight. H2O was added cautiously, and the mixture was extracted with EtOAc (3×200 mL). The combined extracts were washed with brine, dried (MgSO4), and concentrated. The crude 5-(hydroxymethyl)-4-isopropyl-thiazole thus obtained was used as is in the next step.
後処理
- extractionthe mixture was extracted with EtOAc (3×200 mL)
- washThe combined extracts were washed with brine
- dry with materialdried (MgSO4)
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-bf2171462fe843d896eccc484155b9db
- 出典データセット
- uspto-grants-2005_02
- 特許番号
- US06852711B2
反応ノート
読み込み中…