Hydrochloric Acid → 4-(3-Chloro-4-fluoro-phenyl)-6-piperazin-1-yl-2-(4-propyl-piperazin-1-yl)-pyrimidine

HRID 2195071노트

반응식

HRID 2195071 반응식
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:19]=[C:18]([C:20]3[CH:25]=[CH:24][C:23]([F:26])=[C:22]([Cl:27])[CH:21]=3)[N:17]=[C:16]([N:28]3[CH2:33][CH2:32][N:31]([CH2:34][CH2:35][CH3:36])[CH2:30][CH2:29]3)[N:15]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.Cl>O1CCOCC1>[Cl:27][C:22]1[CH:21]=[C:20]([C:18]2[CH:19]=[C:14]([N:11]3[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]3)[N:15]=[C:16]([N:28]3[CH2:29][CH2:30][N:31]([CH2:34][CH2:35][CH3:36])[CH2:32][CH2:33]3)[N:17]=2)[CH:25]=[CH:24][C:23]=1[F:26]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 591683134-[6-(3-Chloro-4-fluoro-phenyl)-2-(4-propyl-piperazin-1-yl)-pyrimidin-4-yl]-piperazine-1-carboxylic acid tert-butyl ester

생성물 1

HCID 591682494-(3-Chloro-4-fluoro-phenyl)-6-piperazin-1-yl-2-(4-propyl-piperazin-1-yl)-pyrimidine

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

Dissolve 4-[6-(3-chloro-4-fluoro-phenyl)-2-(4-propyl-piperazin-1-yl)-pyrimidin-4-yl]-piperazine-1-carboxylic acid tert-butyl ester (2.0 g) in dioxane and then add a 4M solution of HCl in dioxane (15 mL). After the formation of precipitate stir the suspension vigorously for 2 h. Collect the solid and wash with ether and then freebase the material by partitioning between 10% NaOH solution and DCM. Separate the organic layer, dry (Na2SO4) and concentrate to give the title compound as an off-white solid.

후처리

  1. customCollect the solid
  2. washwash with ether
  3. customby partitioning between 10% NaOH solution and DCM
  4. customSeparate the organic layer
  5. dry with materialdry (Na2SO4)
  6. concentrationconcentrate

출처 및 근거

ORD 기록
ord-abb5276e478b4dbe8c39843d36a89128
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08334382B2

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