Hydrochloric Acid → HCID 178522657、化合物

HRID 34961

反応式

HRID 34961 の反応式
Br[C:2]1[C:3](OC(C)C)=[C:4]([CH:8]=[CH:9][C:10]=1OC)[C:5](O)=[O:6].C(N1C=CN=C1)(N1C=CN=C1)=O.[Cl-].[Cl-].[Ca+2].C(N(CC)CC)C.[NH2:39][C:40]1[NH:44][N:43]=[N:42][N:41]=1.Cl>C(#N)C>[NH:41]1[C:40]([NH:39][C:5](=[O:6])[C:4]2[CH:8]=[CH:9][CH:10]=[CH:2][CH:3]=2)=[N:44][N:43]=[N:42]1

参加物

8

反応物 6

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 682631,1'-CarbonyldiimidazoleHCID 5284359Calcium ChlorideHCID 142765153-Bromo-4-methoxy-2-(1-methylethoxy)benzoic acidHCID 178509299HCID 178509299、化合物

生成物 1

HCID 178522657HCID 178522657、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A mixture of 1.28 g (4.43 mmol) 3-bromo-4-methoxy-2-(1-methylethoxy)benzoic acid (prepared in Step 3) and 0.83 g 5.12 g (5.12 mmol) of 1,1'-carbonyldiimidazole in 15 ml of acetonitrile is warmed at reflux under nitrogen atmosphere (or CaCl2 filled drying tube) for one hour. The reaction mixture is treated with 1.07 g (10.62 mmol) of triethylamine and 0.44 g (5.17 mmol) of anhydrous 5-aminotetrazole. The resulting mixture is warmed at reflux for 30 hours. The reaction mixture is then poured onto 180 g of ice water and acidified with aqueous 10% HCl and filtered to give 1.32 g (1.58 theor., 84%) of 3-bromo-4-methoxy-2- 1-methylethoxy)-N-1H-tetrazol-5-ylbenzamide as a white solid having melting point 255°-256° C.

後処理

  1. temperatureis warmed
  2. temperatureat reflux under nitrogen atmosphere
  3. temperatureThe resulting mixture is warmed
  4. temperatureat reflux for 30 hours
  5. filtrationfiltered

出典と根拠

ORDレコード
ord-407b8cae0d874901b9c8ba61bc41af52
出典データセット
uspto-grants-1988_08
特許番号
US04764525

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