Hydrochloric Acid → HCID 68522948, 화합물

HRID 1948930노트

반응식

HRID 1948930 반응식
[Cl:1][C:2]1[C:3]([F:34])=[C:4]([CH:31]=[CH:32][CH:33]=1)[NH:5][C:6]1[C:15]2[C:10](=[CH:11][C:12]([O:29][CH3:30])=[C:13]([O:16][C@@H:17]3[CH2:21][CH2:20][N:19](C(OC(C)(C)C)=O)[CH2:18]3)[CH:14]=2)[N:9]=[CH:8][N:7]=1.Cl>C(#N)C>[ClH:1].[Cl:1][C:2]1[C:3]([F:34])=[C:4]([CH:31]=[CH:32][CH:33]=1)[NH:5][C:6]1[C:15]2[C:10](=[CH:11][C:12]([O:29][CH3:30])=[C:13]([O:16][C@@H:17]3[CH2:21][CH2:20][NH:19][CH2:18]3)[CH:14]=2)[N:9]=[CH:8][N:7]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 68523595HCID 68523595, 화합물

생성물 1

HCID 68522948HCID 68522948, 화합물수율 190.1%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

4-(3-chloro-2-fluoroanilino)-6-[(3R)-1-(tert-butoxycarbonyl)pyrrolidin-3-yloxy]-7-methoxyquinazoline (2.3 g, 4.7 mmole) was dissolved in acetonitrile (35 ml) and hydrogen chloride (4.0M in 1,4-dioxane) (4.7 ml, 18.8 mmole) was added. The mixture was heated to reflux for one hour. After cooling to room temperature, the solid was filtered, washed with acetonitrile and diethylether, and dried under vacuum to give 4-(3-chloro-2-fluoroanilino)-6-[(3R)-pyrrolidin-3-yloxy]-7-methoxyquinazoline hydrochloride as a white solid (1.9 g, 95%); 1H NMR Spectrum (DMSO d6) 2.17-2.29 (m, 1H); 2.34-2.44 (m, 1H); (m, 3H); 3.72-3.84 (m, 1H); 4.00 (s, 3H); 5.44 (m, 1H); 7.31-7.38 (m, 1H); 7.45 (s, 1H); 7.49-7.55 (m, 1H); 7.59-7.65 (m, 1H); 8.67 (s, 1H); 8.80 (s, 1H); 9.43 (br.s 1H); 9.62 (br.s, 1H); 12.25 (br.s, 1H); Mass Spectrum: (M−H)− 387.

후처리

  1. temperatureThe mixture was heated
  2. temperatureto reflux for one hour
  3. filtrationthe solid was filtered
  4. washwashed with acetonitrile and diethylether
  5. customdried under vacuum

출처 및 근거

ORD 기록
ord-a6040238bd6e45d5973e50b500295a44
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08399667B2

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