Triethylamine → HCID 86751125、化合物

HRID 267082

反応式

HRID 267082 の反応式
Cl.[CH:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH:5]=[CH:4][C:3]=1[CH2:12][N:13]1[C:17]([CH2:18][C:19]([OH:21])=O)=[CH:16][N:15]=[CH:14]1.[OH:22][N:23]1[C:28](=O)C2C=CC=CC=2N=N1.Cl.[CH3:35]N(C)CCCN=C=NCC.C(N(CC)CC)C.C(=O)(O)[O-].[Na+]>CN(C)C=O.O>[CH3:35][O:22][N:23]([CH3:28])[C:19](=[O:21])[CH2:18][C:17]1[N:13]([CH2:12][C:3]2[CH:4]=[CH:5][C:6]3[C:11](=[CH:10][CH:9]=[CH:8][CH:7]=3)[CH:2]=2)[CH:14]=[N:15][CH:16]=1

参加物

8

反応物 5

HCID 8471TriethylamineHCID 730263-hydroxy-1,2,3-benzotriazin-4(3H)-oneHCID 516892Sodium BicarbonateHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 702062051-(2-naphthylmethyl)-1H-imidazol-5-ylacetic acid hydrochloride

生成物 1

HCID 86751125HCID 86751125、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 1-(2-naphthylmethyl)-1H-imidazol-5-ylacetic acid hydrochloride (prepared in Example 4, 0.819 mg, 2.70 mmol) in dimethylformamide (15 ml) was added sequentially N, O-dimethylhydroxylamine hydrochloride (293 mg, 3.0 mmol), 3-hydroxy-1,2,3-benzotriazin-4(3H)-one (HOOBT, 489 mg, 3.0 mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDC, 575 mg, 3.0 mmol) and triethylamine (1.67 ml, 12.0 mmol) and the resulting mixture stirred at room temperature for 18 h. Saturated aq. sodium bicarbonate (30 ml) and water (30 ml) were added and the mixture was extracted with methylene chloride (2×50 ml). The combined organic extracts were washed with brine (50 ml) and the solvent evaporated in vacuo. The residue was purified by flash chromatography (2-4% methanol/methylene chloride gradient elution) to provide the title compound as an oil.

後処理

  1. extractionthe mixture was extracted with methylene chloride (2×50 ml)
  2. washThe combined organic extracts were washed with brine (50 ml)
  3. customthe solvent evaporated in vacuo
  4. customThe residue was purified by flash chromatography (2-4% methanol/methylene chloride gradient elution)

出典と根拠

ORDレコード
ord-b1467f2bd5694d53a51470721eae605e
出典データセット
uspto-grants-1997_07
特許番号
US05652257

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