Hydrochloric Acid → 3-(pyrazol-1-yl)-2-methyl-4-(methylsulfonyl)-N-(1-methyltetrazol-5-yl)benzamide

HRID 448849ノート

反応式

HRID 448849 の反応式
S(Cl)(Cl)=O.[N:5]1([C:10]2[C:11]([CH3:23])=[C:12]([CH:16]=[CH:17][C:18]=2[S:19]([CH3:22])(=[O:21])=[O:20])[C:13](O)=[O:14])[CH:9]=[CH:8][CH:7]=[N:6]1.[CH3:24][N:25]1[C:29]([NH2:30])=[N:28][N:27]=[N:26]1.Cl>CN(C1C=CN=CC=1)C.N1C=CC=CC=1.O>[N:5]1([C:10]2[C:11]([CH3:23])=[C:12]([CH:16]=[CH:17][C:18]=2[S:19]([CH3:22])(=[O:21])=[O:20])[C:13]([NH:30][C:29]2[N:25]([CH3:24])[N:26]=[N:27][N:28]=2)=[O:14])[CH:9]=[CH:8][CH:7]=[N:6]1

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 24386Thionyl ChlorideHCID 1384921-methyl-1H-tetrazol-5-amineHCID 666070373-(Pyrazol-1-yl)-2-methyl-4-(methylsulfonyl)benzoic acid

生成物 1

HCID 666067853-(pyrazol-1-yl)-2-methyl-4-(methylsulfonyl)-N-(1-methyltetrazol-5-yl)benzamide

試薬・触媒・溶媒 3

HCID 142844-(Dimethylamino)pyridine触媒HCID 962Water溶媒HCID 1049Pyridine溶媒

実験手順

At RT, 178 mg (1.5 mmol) of thionyl chloride are added to 280 mg (1.0 mmol) of 3-(pyrazol-1-yl)-2-methyl-4-(methylsulfonyl)benzoic acid, 148 mg (1.5 mmol) of 1-methyl-5-aminotetrazole and 12 mg (0.1 mmol) of DMAP in 2 ml of pyridine. The mixture is stirred at RT for 12 h and, after having been checked by LCMS, stirred at 50° C. for 3 h. 0.1 ml of water is then added, the mixture is stirred at RT for 30 min and 2N HCl is added. The product is filtered off with suction and dried. Yield 134 mg (37%).

後処理

  1. stirringstirred at 50° C. for 3 h
  2. stirringthe mixture is stirred at RT for 30 min
  3. filtrationThe product is filtered off with suction
  4. customdried

出典と根拠

ORDレコード
ord-26c8fb94f7d8496aacadce31e78043c7
出典データセット
uspto-grants-2013_07
特許番号
US08481749B2

反応ノート

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