反応式
O=C[C@@H:3]([C@H:5]([C@@H:7]([C@@H:9]([CH2:11][OH:12])[OH:10])[OH:8])O)O.C1C=[N+]([C@@H]2[O:23][C@H:22](COP(OP(OC[C@H]3O[C@@H](N4C5N=CN=C(N)C=5N=C4)[C@H](OP(O)(O)=O)[C@@H]3O)(O)=O)(O)=O)[C@@H](O)[C@H]2O)C=C(C(N)=O)C=1.[Cl-].[K+].[C:63](#N)C>C1(C)C=CC=CC=1>[CH3:22][O:23][C:7]1([O:8][CH3:63])[CH2:5][CH2:3][O:12][CH2:11][C@@H:9]1[OH:10]参加物
反応条件
- 温度
- 30 °C
実験手順
The above organic solution of 4,4-dimethoxydihydro-2H-pyran-3(4H)-one was extracted 3× with phosphate buffered water (0.55 L). To the combined aqueous extracts was added D-glucose (180 g, 100 mmol), and the solution was heated to 30° C. When the solution exceeded 27° C. upon heating B-NADP+(1.60 g, 499 mmol), GDH-103 (1.60 g, 499 mmol), and KRED-130 (1.60 g, 499 mmol) were added and the mixture was stirred for 17 h at 30° C. Potassium chloride (200 g, 2.68 mol) and acetonitrile (1.3 L) were added. After 30 min, the reaction mixture was transferred to 6 L sep funnel and additional MeCN (0.67 L) and toluene (0.87 L) were added. The aqueous layer was back extracted 1× with a mixture of acetonitrile (1.95 L) and toluene (0.65 L), and 1× with acetonitrile (1.5 L). The combined organic extracts were concentrated in vacuo to provide (3S)-4,4-dimethoxytetrahydro-2H-pyran-3-ol.
後処理
- extractionThe above organic solution of 4,4-dimethoxydihydro-2H-pyran-3(4H)-one was extracted 3× with phosphate
- customexceeded 27° C.
- additionKRED-130 (1.60 g, 499 mmol) were added
- waitAfter 30 min
- customthe reaction mixture was transferred to 6 L sep funnel
- extractionThe aqueous layer was back extracted 1×
- additionwith a mixture of acetonitrile (1.95 L) and toluene (0.65 L), and 1× with acetonitrile (1.5 L)
- concentrationThe combined organic extracts were concentrated in vacuo
出典と根拠
- ORDレコード
- ord-3bcdb1fe714c4d80b06e8bec0e453a8b
- 出典データセット
- uspto-grants-2013_02
- 特許番号
- US08383638B2
関連ノート
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