p-Toluenesulfonic acid monohydrate → HCID 68656124, 화합물

HRID 502484노트

반응식

HRID 502484 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][C:10]2[C:19]3[C:14](=[CH:15][C:16]([O:39][CH2:40][CH:41]4[CH2:43][CH2:42]4)=[C:17]([NH:20][C:21](=[O:38])[CH:22]=[CH:23][CH2:24][N:25]([CH2:30][C:31]([O:33][C:34]([CH3:37])(C)[CH3:35])=[O:32])C[C@@H](O)C)[CH:18]=3)[N:13]=[CH:12][N:11]=2)[CH:5]=[CH:6][C:7]=1[F:8].O.C1(C)C=CC(S(O)(=O)=O)=CC=1>C(#N)C>[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][C:10]2[C:19]3[C:14](=[CH:15][C:16]([O:39][CH2:40][CH:41]4[CH2:43][CH2:42]4)=[C:17]([NH:20][C:21](=[O:38])[CH:22]=[CH:23][CH2:24][N:25]4[CH2:35][C@H:34]([CH3:37])[O:33][C:31](=[O:32])[CH2:30]4)[CH:18]=3)[N:13]=[CH:12][N:11]=2)[CH:5]=[CH:6][C:7]=1[F:8]

참가 물질

4

반응물 2

HCID 521998p-Toluenesulfonic acid monohydrate2회HCID 68656862HCID 68656862, 화합물

생성물 1

HCID 68656124HCID 68656124, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of 700 mg of 4-[(3-chloro-4-fluoro-phenyl)amino]-6-[(4-{N-[(tert.butyl-oxycarbonyl)methyl]-N-((S)-2-hydroxy-prop-1-yl)-amino}-1-oxo-2-buten-1-yl)amino]-7-cyclopropylmethoxy-quinazoline and 228 mg of p-toluenesulphonic acid hydrate in 20 ml of acetonitrile is refluxed for five hours. Then a further 200 mg of p-toluenesulphonic acid hydrate are added and the mixture is again refluxed for five hours. For working up the reaction mixture is evaporated to dryness. The flask residue is distributed between ethyl acetate and saturated sodium carbonate solution. The organic phase is separated off, washed with saturated sodium carbonate solution, water and saturated sodium chloride solution, dried over magnesium sulphate and evaporated down. The oily residue is brought to crystallisation by stirring with 15 ml diethyl ether.

후처리

  1. temperatureis refluxed for five hours
  2. temperaturethe mixture is again refluxed for five hours
  3. customis evaporated to dryness
  4. customThe organic phase is separated off
  5. washwashed with saturated sodium carbonate solution, water and saturated sodium chloride solution
  6. dry with materialdried over magnesium sulphate
  7. customevaporated down
  8. customThe oily residue is brought to crystallisation

출처 및 근거

ORD 기록
ord-dc988545248049438a366ffb7080a35b
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07776315B2

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