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1-Methylpiperazine → 2-(3,5-bis-trifluoromethyl-phenyl)-N-methyl-N-[2-methyl-6'-(4-methyl-piperazin-1-yl)-[3,4']bipyridinyl-3'-yl]-isobutyramide

HRID 347685
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HRID 347685 반응식
[F:1][C:2]([F:35])([F:34])[C:3]1[CH:4]=[C:5]([C:13]([CH3:33])([CH3:32])[C:14]([N:16]([C:18]2[CH:19]=[N:20][C:21](Cl)=[CH:22][C:23]=2[C:24]2[C:25]([CH3:30])=[N:26][CH:27]=[CH:28][CH:29]=2)[CH3:17])=[O:15])[CH:6]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:8]=1.[CH3:36][N:37]1[CH2:42][CH2:41][NH:40][CH2:39][CH2:38]1>CN(C1C=CN=CC=1)C.COC(C)(C)C>[F:1][C:2]([F:35])([F:34])[C:3]1[CH:4]=[C:5]([C:13]([CH3:33])([CH3:32])[C:14]([N:16]([CH3:17])[C:18]2[CH:19]=[N:20][C:21]([N:40]3[CH2:41][CH2:42][N:37]([CH3:36])[CH2:38][CH2:39]3)=[CH:22][C:23]=2[C:24]2[C:25]([CH3:30])=[N:26][CH:27]=[CH:28][CH:29]=2)=[O:15])[CH:6]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:8]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 531671-MethylpiperazineHCID 210836352-(3,5-Bis-trifluoromethyl-phenyl)-N-(6'-chloro-2-methyl-[3,4]bipyridinyl-3'-yl)-N-methyl-isobutyramide

생성물 1

HCID 115560662-(3,5-bis-trifluoromethyl-phenyl)-N-methyl-N-[2-methyl-6'-(4-methyl-piperazin-1-yl)-[3,4']bipyridinyl-3'-yl]-isobutyramide

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매
HCID 15413
tert-Butyl methyl ether
용매

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온도
140 °C

실험 절차

A mixture of 2-(3,5-bis-trifluoromethyl-phenyl)-N-(6′-chloro-2-methyl-[3,4′]bipyridinyl-3′-yl)-N-methyl-isobutyramide, 1-methylpiperazine and 4-(N,N-dimethylamino)pyridine is heated at about 140° C. over night. After cooling to room temperature the mixture is diluted with tert-butyl methyl ether and washed with water. The aqueous layer is extracted with tert-butyl methyl ether. The combined organic layers are dried and concentrated to give the compound 2-(3,5-Bis-trifluoromethyl-phenyl)-N-methyl-N-[2-methyl-6′-(4-methyl-piperazin-1-yl)-[3,4′]bipyridinyl-3′-yl]-isobutyramide of formula I-2.

후처리

  1. temperatureAfter cooling to room temperature the mixture
  2. washwashed with water
  3. extractionThe aqueous layer is extracted with tert-butyl methyl ether
  4. customThe combined organic layers are dried
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-76e228f28cf342bc8080a3ded52eb92c
출처 데이터셋
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07176205B2

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