Methanol → HCID 54335129、化合物
反応式
O[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)=[O:4].[F:11][C:12]1[CH:13]=[C:14]([CH:17]=[CH:18][C:19]=1[F:20])[CH:15]=O.C[O-:22].[Na+].CO>C(OC)(OC)OC>[F:11][C:12]1[CH:13]=[C:14]([CH:15]=[CH:2][C:3]([C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:10]=2[OH:22])=[O:4])[CH:17]=[CH:18][C:19]=1[F:20]参加物
6
実験手順
A mixture of 2-hydroxyacetophenone on Wang resin (2.0 g, 1.76 mmol) was swelled in trimethyl orthoformate (20 mL) for 10 min. 3,4-Difluorobenzaldehyde (6.0 mmol) was added and 25% NaOMe in MeOH (0.86 g, 4.0 mmol) was added to the mixture dropwise over 30 min. The mixture was then stirred for an additional 0.5 h. The resin was filtered and washed with alternating MeOH and CH2Cl2 (×5) and dried under high vacuum overnight to give 2.17 g of 3-(3,4-difluorophenyl)-1-(2-hydroxyphenyl)-2-propen-1-one on Wang resin.
後処理
- filtrationThe resin was filtered
- washwashed with alternating MeOH and CH2Cl2 (×5)
- customdried under high vacuum overnight
出典と根拠
- ORDレコード
- ord-1f04fad7e51048bb9f00dac5369e5540
- 出典データセット
- uspto-grants-2002_05
- 特許番号
- US06384057B1
反応ノート
読み込み中…