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Acetic Acid → (+/-)-5-(7-Chloro-2-(1,3,4-thiadiazolylthio)-4H-benzo[5,6]cyclohepta[1,2-d]thiazol-4-yl)-1-methyl-2,4(1H,3H)-pyrimidinedione

HRID 324508
ノート
印刷プレビュー

反応式

HRID 324508 の反応式
Cl[C:2]1[S:3][C:4]2[CH:11]=[CH:10][C:9]3[CH:12]=[C:13]([Cl:16])[CH:14]=[CH:15][C:8]=3[CH:7]([C:17]3[C:18](=[O:25])[NH:19][C:20](=[O:24])[N:21]([CH3:23])[CH:22]=3)[C:5]=2[N:6]=1.[SH:26][C:27]1[S:28][CH:29]=[N:30][N:31]=1.[H-].[Na+].C(O)(=O)C>CN(C)C=O.O>[Cl:16][C:13]1[CH:14]=[CH:15][C:8]2[CH:7]([C:17]3[C:18](=[O:25])[NH:19][C:20](=[O:24])[N:21]([CH3:23])[CH:22]=3)[C:5]3[N:6]=[C:2]([S:26][C:27]4[S:28][CH:29]=[N:30][N:31]=4)[S:3][C:4]=3[CH:11]=[CH:10][C:9]=2[CH:12]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 176Acetic AcidHCID 24758Sodium hydrideHCID 70113243(+/-)-5-(2,7-Dichloro-4H-benzo[5,6]cyclohepta[1,2-d]thiazol-4-yl)-1-methyl-2,4(1H,3H)-pyrimidinedioneHCID 178527973HCID 178527973、化合物

生成物 1

HCID 70113211(+/-)-5-(7-Chloro-2-(1,3,4-thiadiazolylthio)-4H-benzo[5,6]cyclohepta[1,2-d]thiazol-4-yl)-1-methyl-2,4(1H,3H)-pyrimidinedione

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
55 °C

実験手順

To a mixture of the product from example 44 step (viii) (0.20 g) and 2-mercapto-1,3,4-thiadiazole (0.120 g) in dry dimethylformamide (2 ml) was added 60% sodium hydride (0.041 g). The mixture was stirred for 16 h then heated at 55° C. for 24 h. The reaction mixture was diluted with water and neutralised by the addition of acetic acid. The aqueous was extracted with dichloromethane and the combined organic extracts were dried (MgSO4). The solvent was removed under reduced pressure and the residue purified by flash chromatography eluting with dichloromethane/5% ethanol.

後処理

  1. extractionThe aqueous was extracted with dichloromethane
  2. dry with materialthe combined organic extracts were dried (MgSO4)
  3. customThe solvent was removed under reduced pressure
  4. customthe residue purified by flash chromatography
  5. washeluting with dichloromethane/5% ethanol

出典と根拠

ORDレコード
ord-41069b28a3854e989e612c79d92963e9
出典データセット
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06218376B1

反応ノート

読み込み中…

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