Ethanol → 2,3,8,9-Tetrahydro-5-(4-methoxy-2,3-dimethylphenyl)-9-[(4-methoxy-2,3-dimethylphenyl)-methylene]-5H,6H-pyrano[4,3-d]thiazolo[3,2-a]pyrimidine

HRID 65675

反応式

HRID 65675 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH:9]=[C:10]2[C:15](=O)[C:14](=[CH:17][C:18]3[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[C:20]([CH3:26])[C:19]=3[CH3:27])[CH2:13][O:12][CH2:11]2)=[C:5]([CH3:28])[C:4]=1[CH3:29].[NH2:30][C:31]1[S:32][CH2:33][CH2:34][N:35]=1.CCO>C(Cl)(Cl)Cl>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH:9]2[N:35]3[CH2:34][CH2:33][S:32][C:31]3=[N:30][C:15]3[C:14](=[CH:17][C:18]4[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[C:20]([CH3:26])[C:19]=4[CH3:27])[CH2:13][O:12][CH2:11][C:10]2=3)=[C:5]([CH3:28])[C:4]=1[CH3:29]

参加物

5

反応物 3

HCID 702EthanolHCID 156894,5-Dihydro-2-thiazolamineHCID 54006504Tetrahydro-3,5-bis[(4-methoxy-2,3-dimethylphenyl)methylene]-4H-pyran-4-one

生成物 1

HCID 217866812,3,8,9-Tetrahydro-5-(4-methoxy-2,3-dimethylphenyl)-9-[(4-methoxy-2,3-dimethylphenyl)-methylene]-5H,6H-pyrano[4,3-d]thiazolo[3,2-a]pyrimidine収率 74.5%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

A stirred solution of tetrahydro-3,5-bis[(4-methoxy-2,3-dimethylphenyl)methylene]-4H-pyran-4-one (3.0 g, 7.6 mmole) and 2-amino-2-thiazoline (1.0 g, 9.7 mmole) in 75 ml of CHCl3 is heated at reflux temperature for 72 hours. After cooling, the solution is filtered to remove a small amount of insoluble material. The solvent is evaporated to give an oily residue. Trituration with warm EtOH yields 2.7 g of a yellow solid, m.p. 226°-228° d. Crystallization from 15 ml of DMF gives 2.3 g (63%) of cream colored product, m.p. 235°-237°.

後処理

  1. temperatureat reflux temperature for 72 hours
  2. temperatureAfter cooling
  3. filtrationthe solution is filtered
  4. customto remove a small amount of insoluble material
  5. customThe solvent is evaporated
  6. customto give an oily residue

出典と根拠

ORDレコード
ord-0216767bb51d4822929f14d5e9fea3a9
出典データセット
uspto-grants-1978_12
特許番号
US04128648

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