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Butylamine → 2-amino-5-{3-[(butylamino)methyl]phenyl}-5-[4-(difluoro-methoxy)phenyl]-3-methyl-3,5-dihydro-4H-imidazol-4-one

HRID 2240975
ノート
印刷プレビュー

反応式

HRID 2240975 の反応式
[NH2:1][C:2]1[N:3]([CH3:26])[C:4](=[O:25])[C:5]([C:17]2[CH:18]=[C:19]([CH:22]=[CH:23][CH:24]=2)[CH:20]=O)([C:7]2[CH:12]=[CH:11][C:10]([O:13][CH:14]([F:16])[F:15])=[CH:9][CH:8]=2)[N:6]=1.[CH2:27]([NH2:31])[CH2:28][CH2:29][CH3:30].[BH4-].[Na+].[OH-].[Na+]>CO>[NH2:1][C:2]1[N:3]([CH3:26])[C:4](=[O:25])[C:5]([C:17]2[CH:24]=[CH:23][CH:22]=[C:19]([CH2:20][NH:31][CH2:27][CH2:28][CH2:29][CH3:30])[CH:18]=2)([C:7]2[CH:8]=[CH:9][C:10]([O:13][CH:14]([F:15])[F:16])=[CH:11][CH:12]=2)[N:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8007ButylamineHCID 14798Sodium HydroxideHCID 4311764Sodium borohydrideHCID 16113437HCID 16113437、化合物

生成物 1

HCID 251282652-amino-5-{3-[(butylamino)methyl]phenyl}-5-[4-(difluoro-methoxy)phenyl]-3-methyl-3,5-dihydro-4H-imidazol-4-one収率 75%

試薬・触媒・溶媒 1

HCID 887
Methanol
溶媒

実験手順

A small vial (10 ml) was charged with 3-[2-Amino-4-(4-difluoromethoxy-phenyl)-1-methyl-5-oxo-4,5-dihydro-1H-imidazol-4-yl]-benzaldehyde (90 mg, 250 μmol) and methanol (2 ml). To this was added butylamine (20 mg, 273 μmol). After stirring overnight at room temperature sodium borohydride (24 mg) was added, then after another 4 hours 1N sodium hydroxide (1 ml) was added and the mixture extracted with diethyl ether. The ethereal layer was concentrated by rotary evaporation, diluted with methanol and re-concentrated (repeated three times). Finally the oily residue was redissolved in diethylether/hexanes and concentrated, twice then placed under vacuum to give a white foam 78 mg (75%). 1H NMR (400 MHz, DMSO-d6) δ ppm 0.76-0.83 (m, 3H) 1.21 (quin, J=7.9 Hz, 2H) 1.31 (quin, J=6.3 Hz, 2H) 2.38 (t, J=7.0 Hz, 2H) 2.93 (s, 3H) 3.56 (s, 2H) 6.61 (br. s., 4H) 6.67 (br. s., 1H) 7.04 (d, J=8.8 Hz, 2H) 7.12 (t, J=74.18 Hz, 1H) 7.13-7.27 (m, 3H) 7.37 (s, 1H) 7.42 (d, J=8.8 Hz, 2H); MS (APPI) m/z 417 [M+H]+

後処理

  1. additionwas added
  2. extractionthe mixture extracted with diethyl ether
  3. concentrationThe ethereal layer was concentrated by rotary evaporation
  4. additiondiluted with methanol
  5. concentrationre-concentrated (repeated three times)
  6. dissolutionFinally the oily residue was redissolved in diethylether/hexanes
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-54944d8e00e340458ba481394d11c0c5
出典データセット
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07723368B2

反応ノート

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