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Hydrochloric Acid → [4-(3-Pyrimidylcarboxyamino)-2-phenylbenzoyl]methionine methyl ester

HRID 383126
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HRID 383126 반응식
C[O:2][C:3](N1C=CC=NC1)=[O:4].[OH-].[Na+].Cl.Cl.[CH3:15][O:16][C:17](=[O:39])[C@H:18]([CH2:35][CH2:36][S:37][CH3:38])[NH:19][C:20](=[O:34])[C:21]1[CH:26]=[CH:25][C:24]([NH2:27])=[CH:23][C:22]=1[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1.ON1C(=O)C2C=CC=CC=2N=N1.CN(C)CC[CH2:56][N:57]=[C:58]=[N:59][CH2:60][CH3:61].C(N(CC)CC)C>C1COCC1.C(OCC)(=O)C>[CH3:15][O:16][C:17](=[O:39])[C@H:18]([CH2:35][CH2:36][S:37][CH3:38])[NH:19][C:20](=[O:34])[C:21]1[CH:26]=[CH:25][C:24]([N:27]([N:57]2[CH:56]=[CH:61][CH:60]=[N:59][CH2:58]2)[C:3]([OH:4])=[O:2])=[CH:23][C:22]=1[C:28]1[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=1
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참가 물질

10

반응물 7

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 730263-hydroxy-1,2,3-benzotriazin-4(3H)-oneHCID 69612387(4-Amino-2-phenylbenzoyl)methionine methyl ester hydrochloride2회
HCID 70212497
3-Pyrimidinecarboxylic acid methyl ester

생성물 1

HCID 69845184[4-(3-Pyrimidylcarboxyamino)-2-phenylbenzoyl]methionine methyl ester수율 41%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

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온도
60 °C

실험 절차

A mixture of the 5-pyrimidinecarboxylic acid methyl ester prepared in Example 219A (682 mg, 4.94 mmol) and aqueous sodium hydroxide solution (4.0 M, 2.5 mL) in THF was heated at 60° C. for 1.5 hours. Hydrochloric acid (6.0 N, 2 mL) was added to the reaction mixture, and the solvent was evaporated in vacuo. The residue was dried under high vacuum at 50° C. for 1 hour, and the redesolved in to THF. To the acid solution was added (4-amino-2-phenylbenzoyl)methionine methyl ester (compound 8, 1.97 g, 5.0 mmol), 3-hydroxy 1,2,3-benzotriazin-4(3H)-one (0.978 g, 6.0 mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide (1.15 g, 6.0 mmol) and triethylamine (2.8 mL, 20 mmol). After 14 hours, the reaction mixture was diluted with ethyl acetate (100 mL), washed with water and brine, dried over anhydrous magnesium sulfate, filtered, and concentrated in vacuo. The residue was then purified by column chromatography (50% ethyl acetate-hexane, then ethyl acetate) to give [4-(3-pyrimidylcarboxyamino)-2-phenylbenzoyl]methionine methyl ester (0.937 g, 41%).

후처리

  1. customthe solvent was evaporated in vacuo
  2. customThe residue was dried under high vacuum at 50° C. for 1 hour
  3. washwashed with water and brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe residue was then purified by column chromatography (50% ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-5ffb306a633444b48646a6b11235b4b1
출처 데이터셋
uspto-grants-2001_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06310095B1

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