1,1'-Carbonyldiimidazole → Ethyl 2-amino-2-(4-trifluormethyl-3-pyridinecarbonyloxyimino)-acetate

HRID 1978984

반응식

HRID 1978984 반응식
[C:1]([N:8]1C=CN=C1)([N:3]1C=CN=C1)=O.[F:13][C:14]([F:25])([F:24])[C:15]1[CH:20]=[CH:19][N:18]=[CH:17][C:16]=1[C:21]([OH:23])=[O:22].[CH2:26]([O:28][C:29](NC=NO)=[O:30])[CH3:27]>O1CCOCC1>[NH2:8][C:1](=[N:3][O:22][C:21]([C:16]1[CH:17]=[N:18][CH:19]=[CH:20][C:15]=1[C:14]([F:13])([F:24])[F:25])=[O:23])[C:29]([O:28][CH2:26][CH3:27])=[O:30]

참가 물질

5

반응물 3

HCID 682631,1'-CarbonyldiimidazoleHCID 27775493-Pyridinecarboxylic acid, 4-(trifluoromethyl)-HCID 136108985Ethoxycarbonylformamide oxime

생성물 1

HCID 73994277Ethyl 2-amino-2-(4-trifluormethyl-3-pyridinecarbonyloxyimino)-acetate

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

17.3 g of carbonyidiimidazole are initially charged in 200 ml of 1,4-dioxane and, a little at a time, admixed with 20 g of 4-trifluoromethyl-3-pyridinecarboxylic acid. The mixture is stirred at room temperature for 1 h and subsequently heated to 45° C. for 2 h. After cooling to 30° C., 14.5 g of ethoxycarbonylformamide oxime are added and the mixture is stirred at 45° C. for 3 h. The precipitated solid is filtered off with suction and the filtrate is concentrated to 50 ml and, together with the solid, added to 250 ml of ice-water. The solid is filtered off with suction and dried at 50° C. under reduced pressure. This gives 28.7 g of the product as a white solid of mp. 172-174° C.

후처리

  1. temperaturesubsequently heated to 45° C. for 2 h
  2. temperatureAfter cooling to 30° C.
  3. stirringthe mixture is stirred at 45° C. for 3 h
  4. filtrationThe precipitated solid is filtered off with suction
  5. concentrationthe filtrate is concentrated to 50 ml and, together with the solid
  6. additionadded to 250 ml of ice-water
  7. filtrationThe solid is filtered off with suction
  8. customdried at 50° C. under reduced pressure

출처 및 근거

ORD 기록
ord-0796637d1f214032bedd7a3eb5fa0941
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06239160B1

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