Chlorobenzene → 2-benzylthio-7-hydroxy-6-methyl-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one

HRID 703828

反応式

HRID 703828 の反応式
[NH2:1][C:2]1[S:3][C:4]([S:7][CH2:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[N:5][N:6]=1.[CH3:15][CH:16]([C:29](OC1C(Cl)=CC(Cl)=CC=1Cl)=[O:30])[C:17](OC1C(Cl)=CC(Cl)=CC=1Cl)=[O:18].ClC1C=CC=CC=1>CCCCCC>[CH2:8]([S:7][C:4]1[S:3][C:2]2=[N:1][C:29]([OH:30])=[C:16]([CH3:15])[C:17](=[O:18])[N:6]2[N:5]=1)[C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1

参加物

5

反応物 3

HCID 7964ChlorobenzeneHCID 992851,3,4-Thiadiazol-2-amine, 5-((phenylmethyl)thio)-HCID 12320374Bis(2,4,6-trichlorophenyl) methylpropanedioate

生成物 1

HCID 1360876612-benzylthio-7-hydroxy-6-methyl-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one収率 91%

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

実験手順

A mixture of 19.3 g of 2-amino-5-benzylthio-1,3,4-thiadiazole, 41.3 g of bis(2,4,6-trichlorophenyl) 2-methylmalonate and 60 ml of chlorobenzene was stirred at 135°-140° C. for 1 hour. After cooling, n-hexane was added to the reaction mixture and the formed precipitate was separated by filtration. The separated precipitate was washed with n-hexane and thus 23.9 g of 2-benzylthio-7-hydroxy-6-methyl-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one was obtained. m.p. 247°-250° C. Yield 91%.

後処理

  1. temperatureAfter cooling
  2. customthe formed precipitate was separated by filtration
  3. washThe separated precipitate was washed with n-hexane

出典と根拠

ORDレコード
ord-5754043e082043a497ebabbfb9547b00
出典データセット
uspto-grants-1991_01
特許番号
US04985432

関連ノート

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