Hydrochloric Acid → 1-methyl-2-((2R)-2-methyl-piperazin-1-yl)-1H-[4,4']bipyrimidinyl-6-one

HRID 1045692노트

반응식

HRID 1045692 반응식
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[N:15]([CH3:27])[C:16](=[O:26])[CH:17]=[C:18]([C:20]3[CH:25]=[CH:24][N:23]=[CH:22][N:21]=3)[N:19]=2)[C@H:10]([CH3:28])[CH2:9]1)=O)(C)(C)C.Cl>C(OCC)(=O)C>[CH3:27][N:15]1[C:16](=[O:26])[CH:17]=[C:18]([C:20]2[CH:25]=[CH:24][N:23]=[CH:22][N:21]=2)[N:19]=[C:14]1[N:11]1[CH2:12][CH2:13][NH:8][CH2:9][C@H:10]1[CH3:28]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 57870141(3R)-3-methyl-4-(1-methyl-6-oxo-1,6-dihydro-[4,4']bipyrimidinyl-2-yl)-piperazine-1-carboxylic acid tert-butyl ester

생성물 1

HCID 250045961-methyl-2-((2R)-2-methyl-piperazin-1-yl)-1H-[4,4']bipyrimidinyl-6-one수율 91%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

To a solution of (3R)-3-methyl-4-(1-methyl-6-oxo-1,6-dihydro-[4,4′]bipyrimidinyl-2-yl)-piperazine-1-carboxylic acid tert-butyl ester (6.9 g, 18 mmol) in ethyl acetate (35 ml) was added hydrogen chloride (4N) in ethyl acetate (35 ml) at room temperature. The mixture was stirred at room temperature for 2 hours and was concentrated under reduced pressure. The residue was partitioned between aqueous sodium hydrogen carbonate and chloroform, and the organic layer was dried over sodium sulfate. The solvent was evaporated under reduced pressure to afford 1-methyl-2-((2R)-2-methyl-piperazin-1-yl)-1H-[4,4′]bipyrimidinyl-6-one (4.6 g, 91%).

후처리

  1. concentrationwas concentrated under reduced pressure
  2. customThe residue was partitioned between aqueous sodium hydrogen carbonate and chloroform
  3. dry with materialthe organic layer was dried over sodium sulfate
  4. customThe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-eb473c79e5984026af4910fb632d4ed7
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08569294B2

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