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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
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HRID 1867692 반응식
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
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참가 물질

8

반응물 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

생성물 1

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

시약·촉매·용매 2

HCID 887Methanol용매HCID 3283Diethyl Ether용매

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온도
40 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f414524e5ca64d4cb26d748f0ea137a1
출처 데이터셋
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07632840B2

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