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Triphenylphosphine → 1-(2-Ethyl-1-methyl-1H-benzimidazol-6-yl)-4-((4-(trifluoromethyl)-2-thienyl)methoxy)pyridin-2(1H)-one

HRID 2203103
ノート
印刷プレビュー

反応式

HRID 2203103 の反応式
[F:1][C:2]([F:11])([F:10])[C:3]1[CH:4]=[C:5]([CH2:8][OH:9])[S:6][CH:7]=1.[CH2:12]([C:14]1[N:18]([CH3:19])[C:17]2[CH:20]=[C:21]([N:24]3[CH:29]=[CH:28][C:27](O)=[CH:26][C:25]3=[O:31])[CH:22]=[CH:23][C:16]=2[N:15]=1)[CH3:13].N(C(OCCOC)=O)=NC(OCCOC)=O.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>C1COCC1.O>[CH2:12]([C:14]1[N:18]([CH3:19])[C:17]2[CH:20]=[C:21]([N:24]3[CH:29]=[CH:28][C:27]([O:9][CH2:8][C:5]4[S:6][CH:7]=[C:3]([C:2]([F:10])([F:1])[F:11])[CH:4]=4)=[CH:26][C:25]3=[O:31])[CH:22]=[CH:23][C:16]=2[N:15]=1)[CH3:13]
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 4

HCID 11776TriphenylphosphineHCID 533844152-methoxyethyl N-(2-methoxyethoxycarbonylimino)carbamateHCID 896902462-Thiophenemethanol, 4-(trifluoromethyl)-HCID 896909981-(2-Ethyl-1-methyl-1H-benzimidazol-6-yl)-4-hydroxypyridin-2(1H)-one

生成物 1

HCID 896911371-(2-Ethyl-1-methyl-1H-benzimidazol-6-yl)-4-((4-(trifluoromethyl)-2-thienyl)methoxy)pyridin-2(1H)-one
収率 8.6%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of (4-(trifluoromethyl)thiophen-2-yl)methanol (50 mg) in THF (3 ml) were added 1-(2-ethyl-1-methyl-1H-benzo[d]imidazol-6-yl)-4-hydroxypyridin-2(1H)-one (73.9 mg), bis(2-methoxyethyl) azodicarboxylate (129 mg) and PPh3 (144 mg) at room temperature, and the mixture was stirred for 3 h. The mixture was poured into water and extracted with EtOAc. The organic layer was separated, washed with saturated NaHCO3 solution and brine successively, dried over MgSO4 and concentrated in vacuo. The residue was purified by column chromatography (EtOAc/MeOH) to give the title compound (10.2 mg) as white crystals.

後処理

  1. extractionextracted with EtOAc
  2. customThe organic layer was separated
  3. washwashed with saturated NaHCO3 solution and brine successively
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by column chromatography (EtOAc/MeOH)

出典と根拠

ORDレコード
ord-90a9a1b6cb68402781c807ab66e7f61c
出典データセット
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09365540B2

反応ノート

読み込み中…

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