N-Phenyl diethanolamine → 6-Phenyl-1,3,6-dioxazocan-2-one
反応式
[C:1]1([N:7]([CH2:11][CH2:12][OH:13])[CH2:8][CH2:9][OH:10])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(N(CC)CC)C.Cl[C:22](Cl)([O:24]C(=O)OC(Cl)(Cl)Cl)Cl>C1COCC1>[C:1]1([N:7]2[CH2:11][CH2:12][O:13][C:22](=[O:24])[O:10][CH2:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1参加物
5
実験手順
The procedure of Example 1 was followed using N-phenyldiethanolamine (15.2 g, 83.9 mmol), triethylamine (24.0 mL, 167.8 mmol), dry THF (600 mL) and triphosgene (8.3 g, 28.8 mmol). The filtrate was concentrated yielding a clear oil containing a mixture of products. The product was purified using a column chromatography EtOAc:Hexanes (3:1) yielding 3.3 g (19%) of a clear oil which turned brown over time.
後処理
- concentrationThe filtrate was concentrated
- customyielding a clear oil
- additioncontaining
- additiona mixture of products
- customThe product was purified
出典と根拠
- ORDレコード
- ord-948467aa378f4d8caeda1fd24f843fe1
- 出典データセット
- uspto-grants-2015_12
- 特許番号
- US09215876B2
反応ノート
読み込み中…