Methanol → 3-Thienylglyoxylic acid
反応式
[S:1]1[CH:5]=[CH:4][C:3]([C:6](=[O:12])[C:7]([O:9]CC)=[O:8])=[CH:2]1.[OH-].[Na+].CO>O>[S:1]1[CH:5]=[CH:4][C:3]([C:6](=[O:12])[C:7]([OH:9])=[O:8])=[CH:2]1参加物
5
実験手順
To a mixture of ethyl thien-3-yl-glyoxylate (10 g) and 2 N-sodium hydroxide (50 ml) was added sufficient methanol to produce a homogeneous solution, and the reaction was allowed to stand at room temperature for one hour. The solution was poured into water, extracted with ether, acidified with 2 N-hydrochloric acid and extracted with ether. The combined extracts were dried and evaporated to give an oil which was triturated with benzene-petroleum ether, and the resulting solid filtered and dried (7.5 g; 88%), m.p. 63°, νmax. (Nujol) 3600 and 1702 cm-1 (CO2H), τ (DMSO-d6) values include 1.29, 2.21, 2.38 (thien-3-yl protons).
後処理
- customto produce a homogeneous solution
- extractionextracted with ether
- extractionextracted with ether
- customThe combined extracts were dried
- customevaporated
- customto give an oil which
- customwas triturated with benzene-petroleum ether
- filtrationthe resulting solid filtered
- customdried (7.5 g; 88%), m.p. 63°, νmax
出典と根拠
- ORDレコード
- ord-a676249f34a84418bdbae1124e6573d5
- 出典データセット
- uspto-grants-1980_06
- 特許番号
- US04209616
反応ノート
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