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1-Hydroxybenzotriazole → N-(4-(3-bromophenyl)-3-hydroxybutan-2-yl)-3-(4-(trifluoromethoxy)phenyl)-1,2,4-oxadiazole-5-carboxamide

HRID 517535
ノート
印刷プレビュー

反応式

HRID 517535 の反応式
[F:1][C:2]([F:19])([F:18])[O:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[N:14]=[C:13]([C:15]([O-:17])=O)[O:12][N:11]=2)=[CH:6][CH:5]=1.[Na+].CCN(C(C)C)C(C)C.CCN=C=NCCCN(C)C.Cl.C1C=CC2N(O)N=NC=2C=1.[NH2:52][CH:53]([CH3:64])[CH:54]([OH:63])[CH2:55][C:56]1[CH:61]=[CH:60][CH:59]=[C:58]([Br:62])[CH:57]=1>C(Cl)Cl>[Br:62][C:58]1[CH:57]=[C:56]([CH2:55][CH:54]([OH:63])[CH:53]([NH:52][C:15]([C:13]2[O:12][N:11]=[C:10]([C:7]3[CH:6]=[CH:5][C:4]([O:3][C:2]([F:1])([F:19])[F:18])=[CH:9][CH:8]=3)[N:14]=2)=[O:17])[CH3:64])[CH:61]=[CH:60][CH:59]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 823860203-Amino-1-(3-bromophenyl)butan-2-olHCID 86711476Sodium 3-(4-(trifluoromethoxy)phenyl)-1,2,4-oxadiazole-5-carboxylate

生成物 1

HCID 86711478
N-(4-(3-bromophenyl)-3-hydroxybutan-2-yl)-3-(4-(trifluoromethoxy)phenyl)-1,2,4-oxadiazole-5-carboxamide
収率 41.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of sodium 3-(4-(trifluoromethoxy)phenyl)-1,2,4-oxadiazole-5-carboxylate (500 mg, 1.7 mmol) in DCM (15 mL), DIEA (436 mg, 3.4 mmol), EDC.HCl (496 mg, 2.6 mmol), HOBT (351 mg, 2.6 mmol) and 3-amino-1-(3-bromophenyl)butan-2-ol (500 mg, 2.0 mmol) were added in sequence. The mixture was stirred at RT for 2 h, heated at 40 overnight, cooled to RT, quenched by the addition of H2O (50 mL), and extracted with DCM (50 mL×3). The combined organic layers were washed with H2O (10 mL) and brine (10 mL), dried over Na2SO4, filtered and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (Petroleum ether:EtOAc=5:1) to afford N-(4-(3-bromophenyl)-3-hydroxybutan-2-yl)-3-(4-(trifluoromethoxy)phenyl)-1,2,4-oxadiazole-5-carboxamide (350 mg, 41%) as a white solid. MS (ES+) C20H13BrF3N3O3 requires: 499, 501 found: 500 [M+H]+, 502 [M+2+H]+(1:1).

後処理

  1. temperatureheated at 40 overnight
  2. temperaturecooled to RT
  3. customquenched by the addition of H2O (50 mL)
  4. extractionextracted with DCM (50 mL×3)
  5. washThe combined organic layers were washed with H2O (10 mL) and brine (10 mL)
  6. dry with materialdried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. customThe residue was purified by silica gel column chromatography (Petroleum ether:EtOAc=5:1)

出典と根拠

ORDレコード
ord-4872cf27d17549d8b32050319ac8b826
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09115120B2

反応ノート

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