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Acetic Acid → 6,7-diamino-2-(4-tert-butylphenyl)-5H-[1,3,4]thiadiazolo[3,2-a]pyrimidin-5-one

HRID 1906530
ノート
印刷プレビュー

反応式

HRID 1906530 の反応式
[NH2:1][C:2]1[N:3]=[C:4]2[S:14][C:13]([C:15]3[CH:20]=[CH:19][C:18]([C:21]([CH3:24])([CH3:23])[CH3:22])=[CH:17][CH:16]=3)=[N:12][N:5]2[C:6](=[O:11])[C:7]=1[N+:8]([O-])=O.C(O)(=O)C>CN(C)C=O.[C].[Pd]>[NH2:8][C:7]1[C:6](=[O:11])[N:5]2[N:12]=[C:13]([C:15]3[CH:16]=[CH:17][C:18]([C:21]([CH3:23])([CH3:22])[CH3:24])=[CH:19][CH:20]=3)[S:14][C:4]2=[N:3][C:2]=1[NH2:1]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 176Acetic AcidHCID 135918357-amino-2-(4-tert-butylphenyl)-6-nitro-5H-[1,3,4]thiadiazolo[3,2-a]pyrimidin-5-one

生成物 1

HCID 135918366,7-diamino-2-(4-tert-butylphenyl)-5H-[1,3,4]thiadiazolo[3,2-a]pyrimidin-5-one収率 79.6%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 6228Dimethylformamide溶媒

実験手順

2.75 g of 7-amino-2-(4-tert-butylphenyl)-6-nitro-5H-[1,3,4] thiadiazolo[3,2-a]pyrimidin-5-one was dissolved in 200 ml of warmed dimethylformamide, and 20 ml of acetic acid and 2.0 g of 5% palladium-carbon were added to the solution. Catalytic reduction was carried out at a temperature of 40° to 60° C. After the calculated amount of hydrogen was absorbed, the catalyst was removed by filtration while hot, and the filtrate was concentrated under reduced pressure. The precipitate formed was separated by filtration to obtain 2.0 g of 6,7-diamino-2-(4-tert-butylphenyl)-5H-[1,3,4]thiadiazolo[3,2-a]pyrimidin-5-one as yellow needles.

後処理

  1. customwas carried out at a temperature of 40° to 60° C
  2. customAfter the calculated amount of hydrogen was absorbed
  3. customthe catalyst was removed by filtration while hot, and the filtrate
  4. concentrationwas concentrated under reduced pressure
  5. customThe precipitate formed
  6. customwas separated by filtration

出典と根拠

ORDレコード
ord-141518d4447f4496bf76b1a93cd84951
出典データセット
uspto-grants-1987_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04652646

反応ノート

読み込み中…

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