Hydrochloric Acid → 2-chloro-4-(methylsulfonyl)-N-(1-(2-methoxyethyl)tetrazol-5-yl)-benzamide

HRID 68215ノート

反応式

HRID 68215 の反応式
[Cl:1][C:2]1[CH:10]=[C:9]([S:11]([CH3:14])(=[O:13])=[O:12])[CH:8]=[CH:7][C:3]=1[C:4](Cl)=[O:5].[NH2:15][C:16]1[N:20]([CH2:21][CH2:22][O:23][CH3:24])[N:19]=[N:18][N:17]=1.O.Cl>N1C=CC=CC=1.CC(=O)OCC>[Cl:1][C:2]1[CH:10]=[C:9]([S:11]([CH3:14])(=[O:13])=[O:12])[CH:8]=[CH:7][C:3]=1[C:4]([NH:15][C:16]1[N:20]([CH2:21][CH2:22][O:23][CH3:24])[N:19]=[N:18][N:17]=1)=[O:5]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 11128804Benzoyl chloride, 2-chloro-4-(methylsulfonyl)-HCID 583353441-(2-methoxyethyl)-1H-1,2,3,4-tetrazol-5-amine

生成物 1

HCID 867235572-chloro-4-(methylsulfonyl)-N-(1-(2-methoxyethyl)tetrazol-5-yl)-benzamide

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
60 °C

実験手順

176 mg (0.75 mmol) of 2-chloro-4-(methylsulfonyl)benzoyl chloride, 145 mg (1.0 mmol) of 5-amino-1-(2-methoxyethyl)tetrazole in 2 ml of pyridine are stirred at 60° C. for 12 h. 0.1 ml of water is then added, the mixture is stirred at 60° C. for 30 min and EA and 2N HCl are added. The organic phase is separated off and washed with 2N HCl and brine, dried over Na2SO4, concentrated and purified by RP—HPLC (acetonitrile/water). Yield 66 mg (23%).

後処理

  1. customThe organic phase is separated off
  2. washwashed with 2N HCl and brine
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated
  5. custompurified by RP—HPLC (acetonitrile/water)

出典と根拠

ORDレコード
ord-c8af9790b4d94610883b5f1185ffa93e
出典データセット
uspto-grants-2014_09
特許番号
US08822378B2

反応ノート

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