3-(p-Tolyl)acrylic acid → HCID 66795846、化合物

HRID 500982

反応式

HRID 500982 の反応式
[NH2:1][C:2]([CH3:37])([CH3:36])[CH2:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([NH:11][C:12]2[CH:17]=[CH:16][C:15]([CH2:18][CH2:19][NH:20][CH2:21][C@@H:22]([C:24]3[CH:33]=[CH:32][C:31]([OH:34])=[C:30]4[C:25]=3[CH:26]=[CH:27][C:28](=[O:35])[NH:29]4)[OH:23])=[CH:14][CH:13]=2)=[CH:7][CH:6]=1.[CH3:38][C:39]1[CH:49]=[CH:48][C:42]([CH:43]=[CH:44][C:45]([OH:47])=[O:46])=[CH:41][CH:40]=1>O1CCCC1.O>[CH3:38][C:39]1[CH:49]=[CH:48][C:42]([CH:43]=[CH:44][C:45]([OH:47])=[O:46])=[CH:41][CH:40]=1.[NH2:1][C:2]([CH3:37])([CH3:36])[CH2:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([NH:11][C:12]2[CH:13]=[CH:14][C:15]([CH2:18][CH2:19][NH:20][CH2:21][C@@H:22]([C:24]3[CH:33]=[CH:32][C:31]([OH:34])=[C:30]4[C:25]=3[CH:26]=[CH:27][C:28](=[O:35])[NH:29]4)[OH:23])=[CH:16][CH:17]=2)=[CH:7][CH:6]=1

参加物

5

反応物 2

HCID 158353-(p-Tolyl)acrylic acidHCID 11169365HCID 11169365、化合物

生成物 1

HCID 66795846HCID 66795846、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

5-[(R)-2-(2-{4-[4-(2-amino-2-methyl-propoxy)-phenylamino]-phenyl}-ethylamino)-1-hydroxy-ethyl]-8-hydroxy-1H-quinolin-2-one (0.21 g) was dissolved in a mixture of tetrahydrofuran (1.2 mL) and water (1.2 mL). 4-methyl cinnamic acid (0.07 g, predominantly trans) was added to the stirred solution at room temperature and it dissolved. After approximately 10 minutes, crystallisation occurred. The slurry was stirred overnight and filtered. The cake was washed with aqueous Tetrahydrofuran (1:1 THF:water, 2×0.4 mL, 1×0.2 mL) to afford the title compound which was dried overnight under vacuum at 45° C.

後処理

  1. dissolutionit dissolved
  2. customcrystallisation
  3. filtrationfiltered
  4. washThe cake was washed with aqueous Tetrahydrofuran (1:1 THF:water, 2×0.4 mL, 1×0.2 mL)

出典と根拠

ORDレコード
ord-aacfc98c036b4247b09e5f92a3023509
出典データセット
uspto-grants-2010_08
特許番号
US07772250B2

関連ノート

読み込み中…