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Hydrochloric Acid → 4-(2-Fluoro-5-hydroxy-4-methylanilino)-6-methoxy-7-methoxyacetamidoquinazoline hydrochloride

HRID 634737
ノート
印刷プレビュー

反応式

HRID 634737 の反応式
[OH-].[Na+].[F:3][C:4]1[CH:28]=[C:27]([CH3:29])[C:26]([O:30]C(OC)=O)=[CH:25][C:5]=1[NH:6][C:7]1[C:16]2[C:11](=[CH:12][C:13]([NH:19][C:20](=[O:24])[CH2:21][O:22][CH3:23])=[C:14]([O:17][CH3:18])[CH:15]=2)[N:10]=[CH:9][N:8]=1.[ClH:35]>CO.O>[ClH:35].[F:3][C:4]1[CH:28]=[C:27]([CH3:29])[C:26]([OH:30])=[CH:25][C:5]=1[NH:6][C:7]1[C:16]2[C:11](=[CH:12][C:13]([NH:19][C:20](=[O:24])[CH2:21][O:22][CH3:23])=[C:14]([O:17][CH3:18])[CH:15]=2)[N:10]=[CH:9][N:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 107894254-(2-Fluoro-5-methoxycarbonyloxy-4-methylanilino)-6-methoxy-7-methoxyacetamidoquinazoline

生成物 1

HCID 212602834-(2-Fluoro-5-hydroxy-4-methylanilino)-6-methoxy-7-methoxyacetamidoquinazoline hydrochloride収率 82%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒
HCID 962
Water
溶媒

実験手順

2M Aqueous sodium hydroxide solution (620 μl) was added dropwise to a suspension of 4-(2-fluoro-5-methoxycarbonyloxy-4-methylanilino)-6-methoxy-7-methoxyacetamidoquinazoline (275 mg, 0.62 mmol) in methanol (8 ml) at 5° C. and the mixture then stirred for 90 minutes at ambient temperature. The reaction mixture was diluted with water and adjusted to pH7 with 2M hydrochloric acid. The precipitated solid was collected by filtration, resuspended in ethanol and a 5M solution of hydrogen chloride in isopropanol (0.3 ml) added. The volatiles were removed from the resulting solution by evaporation and the solid washed with ether collected by filtration and dried under vacuum to give 4-(2-fluoro-5-hydroxy-4-methylanilino)-6-methoxy-7-methoxyacetamidoquinazoline hydrochloride (216 mg, 82%).

後処理

  1. filtrationThe precipitated solid was collected by filtration
  2. additiona 5M solution of hydrogen chloride in isopropanol (0.3 ml) added
  3. customThe volatiles were removed from the resulting solution by evaporation
  4. washthe solid washed with ether
  5. filtrationcollected by filtration
  6. customdried under vacuum

出典と根拠

ORDレコード
ord-c83a28a9c46640a182e3a9bcaa415882
出典データセット
uspto-grants-2001_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06184225B2

反応ノート

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