Dimethyl Sulfoxide → HCID 131727715, 화합물

HRID 1432154노트

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HRID 1432154 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:28]=[CH:29][C:30]=1[F:31])[NH:5][C:6]1[C:15]2[C:10](=[CH:11][C:12]([O:26][CH3:27])=[C:13]([O:16][CH2:17][CH2:18][CH2:19][N:20]3[CH2:25][CH2:24][O:23][CH2:22][CH2:21]3)[CH:14]=2)[N:9]=[CH:8][N:7]=1.[CH3:32][S:33]([CH3:35])=[O:34]>C(OCC)(=O)C>[CH3:27][O:26][C:12]1[CH:11]=[C:10]2[N:9]=[CH:8][N:7]=[C:6]([NH:5][C:4]3[CH:28]=[CH:29][C:30]([F:31])=[C:2]([Cl:1])[CH:3]=3)[C:15]2=[CH:14][C:13]=1[O:16][CH2:17][CH2:18][CH2:19][N:20]1[CH2:25][CH2:24][O:23][CH2:22][CH2:21]1.[CH3:32][S:33]([CH3:35])=[O:34]

참가 물질

4

반응물 2

HCID 679Dimethyl SulfoxideHCID 123631Gefitinib

생성물 1

HCID 131727715HCID 131727715, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
75 °C

실험 절차

With warming to about 75° C., 4-(3′-chloro-4′-fluoroanilino)-7-methoxy-6-(3-morpholinopropoxy)quinazoline (204 kg) was dissolved in a mixture of ethyl acetate (1021 liters) and dimethyl sulphoxide (181 liters) containing diatomaceous earth filter aid (5 kg). The resultant mixture was filtered and ethyl acetate (78 liters) was used to wash the filter aid solid. The filtrate and washings were combined and cooled initially to about 10° C. The mixture was then heated to about 40° C. for 1 hour. The warm mixture was cooled to 0° C. at a rate of about 10° C. per hour. The resultant solid was collected by filtration. There was thus obtained Form 3 ZD1839 DMSO solvate as shown by XRPD and DSC analysis.

후처리

  1. additioncontaining diatomaceous earth
  2. filtrationfilter aid (5 kg)
  3. filtrationThe resultant mixture was filtered
  4. washto wash the filter aid solid
  5. temperaturecooled initially to about 10° C
  6. temperatureThe mixture was then heated to about 40° C. for 1 hour
  7. temperatureThe warm mixture was cooled to 0° C. at a rate of about 10° C. per hour
  8. filtrationThe resultant solid was collected by filtration

출처 및 근거

ORD 기록
ord-29301d8c00c240a0985908ab3ea9279a
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07612077B2

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