Triethylamine → HCID 178524952, 화합물

HRID 20325

반응식

HRID 20325 반응식
[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]

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 783922,6-Dichlorobenzoyl chlorideHCID 178470494HCID 178470494, 화합물HCID 178499176HCID 178499176, 화합물

생성물 1

HCID 178524952HCID 178524952, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-779076d1ca1944cca3e65d8e508aefbf
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07745638B2

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