Diethyl (ethoxymethylene)malonate → (S)-Diethyl (7,8-Difluoro-3-Methyl-3,4-Dihydro-2H-[1,4]Benzoxazin-4-Yl)Methylene-Malonate

HRID 8484

反応式

CC(C)([O-])C.[K+].[F:7][C:8]1[CH:18]=[CH:17][C:11]2[NH:12][C@@H:13]([CH3:16])[CH2:14][O:15][C:10]=2[C:9]=1[F:19].C(O[CH:23]=[C:24]([C:30]([O:32][CH2:33][CH3:34])=[O:31])[C:25]([O:27][CH2:28][CH3:29])=[O:26])C>CN(C=O)C>[F:7][C:8]1[CH:18]=[CH:17][C:11]2[N:12]([CH:23]=[C:24]([C:25]([O:27][CH2:28][CH3:29])=[O:26])[C:30]([O:32][CH2:33][CH3:34])=[O:31])[C@@H:13]([CH3:16])[CH2:14][O:15][C:10]=2[C:9]=1[F:19]

参加物

実験手順

To DMF (2.5 ml) was added potassium tertiary-butoxide (75 mg) under ice-cooling. After dropping a solution of the compound (100 mg) obtained in Example 78 and diethyl ethoxymethylenemalonate (233 mg) in DMF (0.5 ml), the resultant mixture was stirred for 2 hours. After treating in a conventional manner, the obtained residue was subjected to silica gel column chromatography to thereby give 153 mg (88%) of the title compound as an oily product. The physical constants of the obtained compounds was identical with those described in Japanese Patent No. 2,769,174.

後処理

temperaturecooling
additionAfter treating in a conventional manner

出典と根拠

ORDレコード: ord-4eb0b563d26541c38317838c6ee3f3f4
出典データセット: uspto-grants-2006_08
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US07087778B2

反応式

参加物

反応物 3

生成物 1

試薬・触媒・溶媒 1

実験手順

後処理

出典と根拠

関連ノート