Hydrochloric Acid → HCID 68522948、化合物

HRID 1948930ノート

反応式

HRID 1948930 の反応式
[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

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 68523595HCID 68523595、化合物

生成物 1

HCID 68522948HCID 68522948、化合物収率 190.1%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a6040238bd6e45d5973e50b500295a44
出典データセット
uspto-grants-2013_03
特許番号
US08399667B2

反応ノート

読み込み中…