Triethylamine → HCID 178524952、化合物

HRID 20325

反応式

HRID 20325 の反応式
[Cl:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([Cl:11])[C:3]=1[C:4](Cl)=[O:5].C[O:13][C:14]([C:16]1[C:20]([NH2:21])=[CH:19][NH:18][N:17]=1)=[O:15].C(OC(C1C(N)=CNN=1)=O)C.C(N(CC)CC)C>O1CCOCC1>[Cl:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([Cl:11])[C:3]=1[C:4]([NH:21][C:20]1[C:16]([C:14]([OH:15])=[O:13])=[N:17][NH:18][CH:19]=1)=[O:5]

参加物

6

反応物 4

HCID 8471TriethylamineHCID 783922,6-Dichlorobenzoyl chlorideHCID 178470494HCID 178470494、化合物HCID 178499176HCID 178499176、化合物

生成物 1

HCID 178524952HCID 178524952、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

2,6-dichlorobenzoyl chloride (8.2 g; 39.05 mmol) was added cautiously to a solution of 4-amino-1H-pyrazole-3-carboxylic acid methyl ester (prepared in a manner analogous to 165B) (5 g; 35.5 mmol) and triethylamine (5.95 ml; 42.6 mmol) in dioxan (50 ml) then stirred at room temperature for 5 hours. The reaction mixture was filtered and the filtrate treated with methanol (50 ml) and 2M sodium hydroxide solution (100 ml), heated at 50° C. for 4 hours, and then evaporated. 100 ml of water was added to the residue then acidified with concentrated hydrochloric acid. The solid was collected by filtration, washed with water (100 ml) and sucked dry to give 10.05 g of 4-(2,6-dichloro-benzoylamino)-1H-pyrazole-3-carboxylic acid as a pale violet solid.

後処理

  1. filtrationThe reaction mixture was filtered
  2. additionthe filtrate treated with methanol (50 ml) and 2M sodium hydroxide solution (100 ml)
  3. temperatureheated at 50° C. for 4 hours
  4. customevaporated
  5. addition100 ml of water was added to the residue
  6. filtrationThe solid was collected by filtration
  7. washwashed with water (100 ml)
  8. customsucked dry

出典と根拠

ORDレコード
ord-779076d1ca1944cca3e65d8e508aefbf
出典データセット
uspto-grants-2010_06
特許番号
US07745638B2

関連ノート

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