Calcium Carbonate → Afatinib Impurity 56

HRID 1929787노트

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HRID 1929787 반응식
[CH3:1][N:2]([CH3:9])[CH2:3][C:4]#[C:5][C:6]([OH:8])=[O:7].C(=O)([O-])[O-].[Ca+2]>C(OCC)(=O)C.CO>[CH3:1][N:2]([CH3:9])[CH2:3]/[CH:4]=[CH:5]\[C:6]([OH:8])=[O:7]

참가 물질

5

반응물 2

HCID 10112Calcium CarbonateHCID 150797524-(Dimethylamino)but-2-ynoic acid

생성물 1

HCID 59504961Afatinib Impurity 56수율 39.4%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8857Ethyl Acetate용매

실험 절차

2 g of the compound obtained in step 1) was diluted with 120 ml of a mixed solvent of ethyl acetate and methanol (1:1), and 450 mg of calcium carbonate on palladium was added thereto. The resulting mixture was stirred under a hydrogen gas for two hours. After the reaction terminated, the resulting solution was filtered through a cellite pad and distilled under a reduced pressure. The resulting residue was purified by column chromatography (methylene chloride:methanol=2:1) to obtain the title compound (800 mg, 39%).

후처리

  1. additionwas added
  2. customAfter the reaction terminated
  3. filtrationthe resulting solution was filtered through a cellite pad
  4. distillationdistilled under a reduced pressure
  5. customThe resulting residue was purified by column chromatography (methylene chloride:methanol=2:1)

출처 및 근거

ORD 기록
ord-e45c468293b94d2e840300a46cbb77cd
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08188102B2

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