4-[(4,5-Dihydro-2-thiazolyl)amino]tetrahydro-3,5-bis[(4-methoxyphenyl)methylene]thiopyran-4-ol-1,1-dioxide → 2,3,8,9-Tetrahydro-5-(4-methoxyphenyl)-9-[(4-methoxyphenyl)methylene]-5H,6H-thiazolo[3,2-a]thiopyrano[4,3-d]pyrimidine-7,7-dioxide

HRID 65668ノート

反応式

HRID 65668 の反応式
[S:1]1[CH2:5][CH2:4][N:3]=[C:2]1[NH:6][C:7]1(O)[C:12](=[CH:13][C:14]2[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=2)[CH2:11][S:10](=[O:23])(=[O:22])[CH2:9][C:8]1=[CH:24][C:25]1[CH:30]=[CH:29][C:28]([O:31][CH3:32])=[CH:27][CH:26]=1>CCCCO.CS(C)=O>[CH3:32][O:31][C:28]1[CH:29]=[CH:30][C:25]([CH:24]2[N:3]3[CH2:4][CH2:5][S:1][C:2]3=[N:6][C:7]3[C:12](=[CH:13][C:14]4[CH:15]=[CH:16][C:17]([O:20][CH3:21])=[CH:18][CH:19]=4)[CH2:11][S:10](=[O:22])(=[O:23])[CH2:9][C:8]2=3)=[CH:26][CH:27]=1

参加物

4

反応物 1

HCID 540765934-[(4,5-Dihydro-2-thiazolyl)amino]tetrahydro-3,5-bis[(4-methoxyphenyl)methylene]thiopyran-4-ol-1,1-dioxide

生成物 1

HCID 217866772,3,8,9-Tetrahydro-5-(4-methoxyphenyl)-9-[(4-methoxyphenyl)methylene]-5H,6H-thiazolo[3,2-a]thiopyrano[4,3-d]pyrimidine-7,7-dioxide

試薬・触媒・溶媒 2

HCID 2631-Butanol溶媒HCID 679Dimethyl Sulfoxide溶媒

実験手順

A suspension of 4-[(4,5-dihydro-2-thiazolyl)amino]-tetrahydro-3,5-bis[(4-methoxyphenyl)methylene]thiopyran-4-ol-1,1-dioxide (6.0 g, 0.012 mole) in 75 ml of n-BuOH and 25 ml of DMSO is stirred and heated at reflux for 1 hour. The volume of the resulting solution is reduced by approximately one-half using a Dean-Stark trap. After cooling, the yield of yellow product is 4.7 g, m.p. 235°-240°. Crystallization from 25 ml of DMF gives 4.0 g (69%) of cream colored product, m.p. 243°-245°.

後処理

  1. temperatureheated
  2. temperatureat reflux for 1 hour
  3. temperatureAfter cooling
  4. customCrystallization from 25 ml of DMF
  5. customgives 4.0 g (69%) of cream colored product, m.p. 243°-245°

出典と根拠

ORDレコード
ord-d525f170739548938a3dae54d1925a5f
出典データセット
uspto-grants-1978_12
特許番号
US04128647

反応ノート

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