Sodium Acetate → HCID 75600536、化合物

HRID 2281028ノート

反応式

HRID 2281028 の反応式
[CH2:1]([N:3]1[C:7](=[S:8])[CH2:6][O:5][C:4]1=[S:9])[CH3:2].[CH3:10][O:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[C:18]1[O:22][C:21]([CH:23]=O)=[CH:20][CH:19]=1.C([O-])(=O)C.[Na+]>C(O)(=O)C>[CH2:1]([N:3]1[C:7](=[S:8])[C:6](=[CH:23][C:21]2[O:22][C:18]([C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=3[O:11][CH3:10])=[CH:19][CH:20]=2)[O:5][C:4]1=[S:9])[CH3:2]

参加物

5

反応物 3

HCID 517045Sodium AcetateHCID 46749915-(2-Methoxyphenyl)-2-furancarboxaldehydeHCID 86676053HCID 86676053、化合物

生成物 1

HCID 75600536HCID 75600536、化合物収率 95%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To a mixture of 3-ethyloxazolidine-2,4-dithione 6 (79 mg, 0.49 mmol), 5-(2-methoxyphenyl)-2-furaldehyde 9 (99 mg, 0.49 mmol) and sodium acetate (201 mg, 2.45 mmol) was added acetic acid (5 mL). As more of the desired product was formed, the reaction mixture color turned to a very red solution. The reaction mixture was refluxed overnight, then the excess solvent was removed in vacuo. The residue was diluted with ethyl acetate (100 mL), then washed with water (2×20 mL). The organic layer was dried with brine and MgSO4, then concentrated in vacuo. Flash column chromatography afforded the desired product 2 (M103) in 95% yield (160 mg, purple solid).

出典と根拠

ORDレコード
ord-bf9f6bc7873a4108a34da8f8d5a4511c
出典データセット
uspto-grants-2015_09
特許番号
US09139575B2

反応ノート

読み込み中…