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3-hydroxy-1,2,3-benzotriazin-4(3H)-one → [4-(3-Pyridyloxymethyl)-2-phenylbenzoyl]alanine methyl ester

HRID 2121166
ノート
印刷プレビュー

反応式

HRID 2121166 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([O:7][CH2:8][C:9]2[CH:17]=[CH:16][C:12]([C:13](O)=[O:14])=[C:11]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[CH:10]=2)[CH:2]=1.Cl.[CH3:25][O:26][C:27](=[O:31])[C@H:28]([CH3:30])[NH2:29].Cl.CN(C)CCCN=C=NCC.ON1C(=O)C2C=CC=CC=2N=N1.C(=O)(O)[O-].[Na+]>CN(C)C=O.C(N(CC)CC)C>[CH3:25][O:26][C:27](=[O:31])[C@H:28]([CH3:30])[NH:29][C:13](=[O:14])[C:12]1[CH:16]=[CH:17][C:9]([CH2:8][O:7][C:3]2[CH:2]=[N:1][CH:6]=[CH:5][CH:4]=2)=[CH:10][C:11]=1[C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1
参加物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 730263-hydroxy-1,2,3-benzotriazin-4(3H)-oneHCID 516892Sodium BicarbonateHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 2733257Alanine methyl ester hydrochlorideHCID 234363704-(3-Pyridyloxymethyl)2-phenylbenzoic acid

生成物 1

HCID 69892498
[4-(3-Pyridyloxymethyl)-2-phenylbenzoyl]alanine methyl ester

試薬・触媒・溶媒 2

HCID 8471Triethylamine触媒HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 100 mg (0.33 mmol) of 4-(3-pyridyloxymethyl)-2-phenylbenzoic acid, L-alanine methyl ester hydrochloride (1.5 mmol), 69 mg (0.36 mmol) of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride, and 59 mg (0.36 mmol) of 3-hydroxy1,2,3-benzotriazin-4(3H)-one in 1 mL of N,N-dimethylformamide was added 5 drops of triethylamine. The mixture was stirred at ambient temperature for 24 hours, then poured into 10 mL of 0.6M aqueous sodium bicarbonate and extracted with ethyl acetate (3×5 mL). The combined ethyl acetate layers were back extracted with water (2×5 mL), then brine (1×5 mL), dried over magnesium sulfate, filtered, and concentrated in vacuo. The product was purified via chromatography over silica gel, eluting with an appropriate mixture of hexanes and ethyl acetate.

後処理

  1. extractionextracted with ethyl acetate (3×5 mL)
  2. extractionThe combined ethyl acetate layers were back extracted with water (2×5 mL)
  3. dry with materialbrine (1×5 mL), dried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe product was purified via chromatography over silica gel
  7. washeluting with an appropriate mixture of hexanes and ethyl acetate

出典と根拠

ORDレコード
ord-7953df887d344e8089af025376627a64
出典データセット
uspto-grants-2004_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06693123B2

反応ノート

読み込み中…

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