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Water → (S)-4-[2-Hydroxy-3-([4-(4-carbamoylphenoxy)phenyl]-2-methylpropylamino)propoxy]carbazole

HRID 1824324
ノート
印刷プレビュー

反応式

HRID 1824324 の反応式
[O:1]1[CH2:3][C@H:2]1[CH2:4][O:5][C:6]1[C:18]2[C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[NH:11][C:10]=2[CH:9]=[CH:8][CH:7]=1.NC(C)(C)C[C:22]1[CH:37]=[CH:36][C:25]([O:26][C:27]2[CH:35]=[CH:34][C:30]([C:31]([NH2:33])=[O:32])=[CH:29][CH:28]=2)=[CH:24][CH:23]=1.O>C(O)(=O)C.CO>[OH:1][C@@H:2]([CH2:3][N:11]([C:22]1[CH:23]=[CH:24][C:25]([O:26][C:27]2[CH:28]=[CH:29][C:30]([C:31](=[O:32])[NH2:33])=[CH:34][CH:35]=2)=[CH:36][CH:37]=1)[CH2:10][CH:18]([CH3:6])[CH3:17])[CH2:4][O:5][C:6]1[C:18]2[C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[NH:11][C:10]=2[CH:9]=[CH:8][CH:7]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 962WaterHCID 10879208(S)-(+)-4-(2,3-Epoxypropoxy)carbazoleHCID 118329614-(4-(2-Amino-2-methylpropyl)phenoxy)benzamide2 回

生成物 1

HCID 53754997(S)-4-[2-Hydroxy-3-([4-(4-carbamoylphenoxy)phenyl]-2-methylpropylamino)propoxy]carbazole収率 174.6%

試薬・触媒・溶媒 2

HCID 176Acetic Acid触媒
HCID 887
Methanol
溶媒

反応条件

温度
60 °C

実験手順

A stirred mixture of (S)-(+)-4-(oxiranylmethoxy)carbazole (7.50 g, 31.3 mmol), 4-(4-(2-amino-2-methylpropyl)-phenoxy)benzamide (17.82 g, 62.67 mmol), acetic acid (0.10 g, 1.7 mmol), water (10 mL) and methanol (260 mL) was heated to 60° C. for 22.7 hrs. The mixture was cooled and concentrated in vacuo to an oil. The concentrate was taken up in ethyl acetate (250 mL) and partitioned with water (100 mL). The organic layer was then extracted with a solution of 25 mL 1N HCl (25 mL) in water (35 mL). A white precipitate formed during the extraction was mostly 4-(4-(2-amino-2-methylpropyl)-phenoxy)benzamide and was removed by filtration of the two phase mixture. The organic layer was extracted two times with a solution of 1N HCl (3 mL) in water (50 mL). The ethyl acetate layer was stripped to an oily residue. The crude product was purified by flash chromatography with 416 g 230–400 silica gel and eluting with ethyl acetate then 10:1–3 ethyl acetate:ethanol gradient. Concentration of the appropriate fractions and drying under vacuum gave 14.31 g (87.2%) of the desired product as a foamy white solid. 1H NMR was consistent with the desired compound.

後処理

  1. temperatureThe mixture was cooled
  2. concentrationconcentrated in vacuo to an oil
  3. custompartitioned with water (100 mL)
  4. extractionThe organic layer was then extracted with a solution of 25 mL 1N HCl (25 mL) in water (35 mL)
  5. customA white precipitate formed during the extraction
  6. customwas removed by filtration of the two phase mixture
  7. extractionThe organic layer was extracted two times with a solution of 1N HCl (3 mL) in water (50 mL)
  8. customThe crude product was purified by flash chromatography with 416 g 230–400 silica gel
  9. washeluting with ethyl acetate
  10. customConcentration of the appropriate fractions and drying under vacuum

出典と根拠

ORDレコード
ord-f92dbe21917e420f80e2ed9ccc609057
出典データセット
uspto-grants-2006_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07041684B2

反応ノート

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