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(Ethoxycarbonylmethyl)triphenylphosphonium bromide → Ethyl (2E)-3-(4-[(3-chloro-4-fluorophenyl)amino]carbonyl-1,2,5-oxadiazol-3-yl)acrylate

HRID 1845785
ノート
印刷プレビュー

反応式

HRID 1845785 の反応式
[Br-].[C:2]([CH2:7][P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)([O:4][CH2:5][CH3:6])=[O:3].CC(C)([O-])C.[Na+].[Cl:33][C:34]1[CH:35]=[C:36]([NH:41][C:42]([C:44]2[C:48]([CH:49]=O)=[N:47][O:46][N:45]=2)=[O:43])[CH:37]=[CH:38][C:39]=1[F:40]>C1(C)C=CC=CC=1.C1COCC1>[Cl:33][C:34]1[CH:35]=[C:36]([NH:41][C:42]([C:44]2[C:48](/[CH:49]=[CH:7]/[C:2]([O:4][CH2:5][CH3:6])=[O:3])=[N:47][O:46][N:45]=2)=[O:43])[CH:37]=[CH:38][C:39]=1[F:40]
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 73731(Ethoxycarbonylmethyl)triphenylphosphonium bromideHCID 23676156Sodium t-butoxideHCID 58941813HCID 58941813、化合物

生成物 1

HCID 58941780Ethyl (2E)-3-(4-[(3-chloro-4-fluorophenyl)amino]carbonyl-1,2,5-oxadiazol-3-yl)acrylate収率 89%

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒
HCID 8028
Tetrahydrofuran
溶媒

反応条件

温度
80 °C

実験手順

To a solution of (carbethoxymethyl)triphenylphosphonium bromide (3.14 g, 7.32 mmol) in toluene (37 mL) was added sodium tert-butoxide (723 mg, 7.52 mmol) at rt under a nitrogen atmosphere. After stirring for 30 min, a solution of N-(3-chloro-4-fluorophenyl)-4-formyl-1,2,5-oxadiazole-3-carboxamide (811 mg, 3.01 mmol) in THF (10 mL) was cannulated into reaction flask. The resulting solution was heated at 80° C. for 3 h, then cooled to rt overnight. The reaction was quenched with a 1 N HCl solution, the aqueous solution was extracted with ethyl acetate. The combined organic solutions were washed with brine, dried over Na2SO4, filtered and concentrate under reduced pressure. The residue was purified with flash chromatography (30% ethyl acetate/hexane) to give the desired product as a white solid (0.91 g, 89%). 1H NMR (400 MHz, CD3OD): δ 7.92 (m, 2 H), 7.65 (m, 1 H), 7.26 (m, 1H), 7.01 (m, 1 H), 4.27 (m, 2 H), 1.33 (m, 3 H); LCMS for C14H12ClFN3O4(M+H)+: m/z=340.

後処理

  1. temperaturecooled to rt overnight
  2. customThe reaction was quenched with a 1 N HCl solution
  3. extractionthe aqueous solution was extracted with ethyl acetate
  4. washThe combined organic solutions were washed with brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrate under reduced pressure
  8. customThe residue was purified with flash chromatography (30% ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-429a24a5c583444b98e7c74891419169
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08951536B2

反応ノート

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