Water → tert-Butyl 4-[7-(2,4-dichlorophenyl)-5-oxo-5,6-dihydro [1,2,4]triazolo[1,5-c]pyrimidin-2-yl]-piperidine-1-carboxylate

HRID 2088676

반응식

HRID 2088676 반응식
[Cl-].[Ca+2].[Cl-].C([O:6][C:7](=O)[NH:8][C:9]([C:13]1[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=1[Cl:20])=[CH:10][C:11]#[N:12])C.[NH:22]([C:24]([CH:26]1[CH2:31][CH2:30][N:29]([C:32]([O:34][C:35]([CH3:38])([CH3:37])[CH3:36])=[O:33])[CH2:28][CH2:27]1)=O)[NH2:23].O>CN1CCCC1=O>[Cl:20][C:14]1[CH:15]=[C:16]([Cl:19])[CH:17]=[CH:18][C:13]=1[C:9]1[NH:8][C:7](=[O:6])[N:23]2[N:22]=[C:24]([CH:26]3[CH2:31][CH2:30][N:29]([C:32]([O:34][C:35]([CH3:38])([CH3:37])[CH3:36])=[O:33])[CH2:28][CH2:27]3)[N:12]=[C:11]2[CH:10]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 5284359Calcium ChlorideHCID 22713165tert-Butyl 4-(hydrazinecarbonyl)piperidine-1-carboxylateHCID 76754608Ethyl[2-cyano-1-(2,4-dichlorophenyl)ethenyl]carbamate

생성물 1

HCID 136104185tert-Butyl 4-[7-(2,4-dichlorophenyl)-5-oxo-5,6-dihydro [1,2,4]triazolo[1,5-c]pyrimidin-2-yl]-piperidine-1-carboxylate

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

반응 조건

온도
150 °C

실험 절차

In a round-bottom flask fitted with reflux condenser and a drying tube filled with calcium chloride, 5.86 g (20.6 mmol) of ethyl[2-cyano-1-(2,4-dichlorophenyl)ethenyl]carbamate and 5.00 g (20.6 mmol) of tert-butyl 4-(hydrazinylcarbonyl)piperidine-1-carboxylate were dissolved in 11 ml of 1-methyl-2-pyrrolidone, and the reaction mixture was stirred at 150° C. for 3 h. The reaction solution was cooled to RT, water (150 ml) was added and the mixture was stirred in an ultrasonic bath for another 2 min. The solid was filtered off with suction and dried under high vacuum. This gave 7.23 g (76% of theory) of the product.

후처리

  1. customIn a round-bottom flask fitted
  2. temperaturewith reflux condenser and a drying tube
  3. temperatureThe reaction solution was cooled to RT
  4. stirringthe mixture was stirred in an ultrasonic bath for another 2 min
  5. filtrationThe solid was filtered off with suction
  6. customdried under high vacuum

출처 및 근거

ORD 기록
ord-0c2b4895ab8e4f2fa572acd5025e5da4
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08436003B2

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