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Acetaldehyde → 4-[({4-[(3-chloro-2-fluorophenyl)amino]-7-methoxyquinazolin-6-yl}methyl)(ethyl)amino]tetrahydro-2H-pyran-4-carboxylic acid

HRID 1867692
ノート
印刷プレビュー

反応式

HRID 1867692 の反応式
Cl.[Cl:2][C:3]1[C:4]([F:33])=[C:5]([NH:9][C:10]2[C:19]3[C:14](=[CH:15][C:16]([O:31][CH3:32])=[C:17]([CH2:20][NH:21][C:22]4([C:28]([OH:30])=[O:29])[CH2:27][CH2:26][O:25][CH2:24][CH2:23]4)[CH:18]=3)[N:13]=[CH:12][N:11]=2)[CH:6]=[CH:7][CH:8]=1.[CH:34](=O)[CH3:35].S([O-])([O-])(=O)=O.[Mg+2].C([BH3-])#N.[Na+]>C(OCC)C.CO>[Cl:2][C:3]1[C:4]([F:33])=[C:5]([NH:9][C:10]2[C:19]3[C:14](=[CH:15][C:16]([O:31][CH3:32])=[C:17]([CH2:20][N:21]([CH2:34][CH3:35])[C:22]4([C:28]([OH:30])=[O:29])[CH2:27][CH2:26][O:25][CH2:24][CH2:23]4)[CH:18]=3)[N:13]=[CH:12][N:11]=2)[CH:6]=[CH:7][CH:8]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 177AcetaldehydeHCID 313Hydrochloric AcidHCID 24083Sulfuric acid magnesium salt (1:1)HCID 5003444Sodium cyanoborohydrideHCID 579798634-[({4-[(3-chloro-2-fluorophenyl)amino]-7-methoxyquinazolin-6-yl}methyl)amino]tetrahydro-2H-pyran-4-carboxylic acid

生成物 1

HCID 57979852
4-[({4-[(3-chloro-2-fluorophenyl)amino]-7-methoxyquinazolin-6-yl}methyl)(ethyl)amino]tetrahydro-2H-pyran-4-carboxylic acid
収率 63%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 3283Diethyl Ether溶媒

反応条件

温度
40 °C

実験手順

1M HCl in diethyl ether (1.4 ml) was added to a stirred suspension of 4-[({4-[(3-chloro-2-fluorophenyl)amino]-7-methoxyquinazolin-6-yl}methyl)amino]tetrahydro-2H-pyran-4-carboxylic acid (0.66 g, 1.43 mmol), acetaldehyde (1.6 ml, 28.6 mmol) and anhydrous magnesium sulfate (0.34 g, 2.83 mmol) in methanol (10 ml). Sodium cyanoborohydride (0.36 g, 5.71 mmol) was added and the resulting mixture heated at 40° C. for 4 hours. The reaction mixture was then filtered and evaporated. The residues were purified by column chromatography on silica, eluting with 7M ammonia in methanol/methylene chloride (16/84). Fractions containing the desired product were combined and evaporated. The resulting gum was triturated with diethyl ether to give 4-[({4-[(3-chloro-2-fluorophenyl)amino]-7-methoxyquinazolin-6-yl}methyl)(ethyl)amino]tetrahydro-2H-pyran-4-carboxylic acid as a white solid (440 mg, 63%); 1H NMR Spectrum: (DMSO-d6) δ 0.79 (t, 3H), 1.71-1.84 (m, 2H), 2.07-2.11 (d, 2H), 2.67-2.76 (q, 2H), 3.23-3.33 (t, 2H), 3.80-3.88 (m, 2H), 3.89-3.95 (m, 5H), 7.16 (s, 1H), 7.22-7.29 (m, 1H), 7.43-7.49 (m, 1H), 7.52-7.57 (dd, 1H), 8.38 (s, 1H), 8.41 (s, 1H); Mass Spectrum: (M+H)+ 489.

後処理

  1. filtrationThe reaction mixture was then filtered
  2. customevaporated
  3. customThe residues were purified by column chromatography on silica
  4. washeluting with 7M ammonia in methanol/methylene chloride (16/84)
  5. additionFractions containing the desired product
  6. customevaporated
  7. customThe resulting gum was triturated with diethyl ether

出典と根拠

ORDレコード
ord-f414524e5ca64d4cb26d748f0ea137a1
出典データセット
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07632840B2

反応ノート

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