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Ethyl Acetate → HCID 68157773、化合物

HRID 1892721
ノート
印刷プレビュー

反応式

HRID 1892721 の反応式
[CH3:1][CH:2]([CH3:30])[CH2:3][CH:4]([C:15]1[CH:20]=[CH:19][C:18]([N:21]2[CH:25]=[C:24]([C:26]([F:29])([F:28])[F:27])[N:23]=[CH:22]2)=[CH:17][CH:16]=1)[O:5][C:6]1[CH:14]=[CH:13][C:9]([C:10](O)=[O:11])=[CH:8][CH:7]=1.Cl.[CH3:32][NH:33]CCC(O)=O.Cl.C(N=C=NCCCN(C)C)C.ON1C2N=CC=CC=2N=N1.[C:61]([O:64][CH2:65]C)(=[O:63])[CH3:62]>ClCCl.C(N(CC)CC)C>[CH3:30][CH:2]([CH3:1])[CH2:3][CH:4]([C:15]1[CH:16]=[CH:17][C:18]([N:21]2[CH:25]=[C:24]([C:26]([F:27])([F:28])[F:29])[N:23]=[CH:22]2)=[CH:19][CH:20]=1)[O:5][C:6]1[CH:14]=[CH:13][C:9]([C:10]([NH:33][CH2:32][CH2:62][C:61]([O:64][CH3:65])=[O:63])=[O:11])=[CH:8][CH:7]=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 8857Ethyl AcetateHCID 181649HOAtHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 457919413-(Methylamino)propanoic acid hydrochlorideHCID 681578284-(3-Methyl-1-(4-(4-(trifluoromethyl)-1H-imidazol-1-yl)phenyl)butoxy)benzoic acid

生成物 1

HCID 68157773
HCID 68157773、化合物
収率 90%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8471Triethylamine溶媒

実験手順

4-(3-Methyl-1-(4-(4-(trifluoromethyl)-1H-imidazol-1-yl)phenyl)butoxy)benzoic acid (65 mg, 0.16 mmol), methyl beta-alanine hydrochloride (31 mg, 0.16 mmol), and triethylamine (0.031 mL) were dissolved in dichloromethane (1 mL). 1-Ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (34 mg, 0.18 mmol) was added. The solution was stirred at room temperature for 15 minutes, and 1-hydroxy-7-azabenzotriazole (34 mg, 0.25 mmol) was then added. The resulting yellow solution was stirred overnight. After 18 hours, the reaction was diluted with ethyl acetate (20 mL) and washed with water (25 mL) and brine (10 mL). The organics were dried over magnesium sulfate, filtered and concentrated. Purification by column chromatography (0-100% ethyl acetate in heptane) gave (+/−)-methyl 3-(4-(3-methyl-1-(4-(4-(trifluoromethyl)-1H-imidazol-1-yl)phenyl)butoxy)benzamido)propanoate (70 mg, 90%). 1H NMR (400 MHz, CDCl3, δ): 7.84 (s, 1H), 7.67-7.62 (m, 2H), 7.58 (s, 1H), 7.53-7.46 (m, 2H), 7.39-7.34 (m 2H), 6.89-6.84 (m, 2H), 6.72 (t, J=5.9 Hz, 1H), 5.29 (dd, J=8.9, 4.5 Hz, 1H), 3.72-3.65 (m, 5H), 2.63 (m, 2H), 2.03 (m, 1H), 1.95-1.83 (m, 1H), 1.65-1.58 (m, 1H), 1.03 (d, J=6.6 Hz, 3H), 0.99 (d, J=6.3 Hz, 3H). MS (M+1): 504.0.

後処理

  1. stirringThe resulting yellow solution was stirred overnight
  2. waitAfter 18 hours
  3. washwashed with water (25 mL) and brine (10 mL)
  4. dry with materialThe organics were dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customPurification by column chromatography (0-100% ethyl acetate in heptane)

出典と根拠

ORDレコード
ord-7a51201a970e44f3b2662e17d4c70eb6
出典データセット
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08507533B2

反応ノート

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