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Dimethylformamide → 5-(Benzo[d][1,3]dioxol-5-yl)-5-methyl-3-[4-[4-propyl-1,1-bis(trifluoromethyl)-1,3-dihydroisobenzofuran-5-yloxy]butyl]imidazolidine-2,4-dione

HRID 552453
ノート
印刷プレビュー

反応式

HRID 552453 の反応式
CN(C)C=O.Br[CH2:7][CH2:8][CH2:9][CH2:10][O:11][C:12]1[C:13]([CH2:29][CH2:30][CH3:31])=[C:14]2[C:18](=[CH:19][CH:20]=1)[C:17]([C:25]([F:28])([F:27])[F:26])([C:21]([F:24])([F:23])[F:22])[O:16][CH2:15]2.C(=O)([O-])[O-].[K+].[K+].[O:38]1[C:42]2[CH:43]=[CH:44][C:45]([C:47]3([CH3:54])[NH:51][C:50](=[O:52])[NH:49][C:48]3=[O:53])=[CH:46][C:41]=2[O:40][CH2:39]1>O>[O:38]1[C:42]2[CH:43]=[CH:44][C:45]([C:47]3([CH3:54])[NH:51][C:50](=[O:52])[N:49]([CH2:7][CH2:8][CH2:9][CH2:10][O:11][C:12]4[C:13]([CH2:29][CH2:30][CH3:31])=[C:14]5[C:18](=[CH:19][CH:20]=4)[C:17]([C:25]([F:28])([F:27])[F:26])([C:21]([F:24])([F:23])[F:22])[O:16][CH2:15]5)[C:48]3=[O:53])=[CH:46][C:41]=2[O:40][CH2:39]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 6228DimethylformamideHCID 11430Potassium CarbonateHCID 28298175-(2H-1,3-benzodioxol-5-yl)-5-methylimidazolidine-2,4-dioneHCID 579007815-(4-Bromobutoxy)-4-propyl-1,1-bis(trifluoromethyl)-1,3-dihydroisobenzofuran

生成物 1

HCID 442412895-(Benzo[d][1,3]dioxol-5-yl)-5-methyl-3-[4-[4-propyl-1,1-bis(trifluoromethyl)-1,3-dihydroisobenzofuran-5-yloxy]butyl]imidazolidine-2,4-dione

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a N,N-Dimethylformamide (2 mL) solution of 5-(4-bromobutoxy)-4-propyl-1,1-bis(trifluoromethyl)-1,3-dihydroisobenzofuran (25 mg, 0.0557 mmol), potassium carbonate mg, 0.111 mmol) and 5-(benzo[d][1,3]dioxol-5-yl)-5-methylimidazolidine-2,4-dione (CAS: 308122-40-9:DE335993) (19.6 mg, 0.0835 mmol) were added and the mixture was stirred overnight. The reaction solution was added with water and extracted with ethyl acetate. Subsequently, the organic layer was washed with saturated saline, dried using anhydrous sodium sulfate, and concentrated in vacuum. The residue was purified by thin-layer silica-gel column chromatography (hexane:ethyl acetate=2:1) and of the title compound (30.7 mg, 92%) was obtained as colorless oil.

後処理

  1. extractionextracted with ethyl acetate
  2. washSubsequently, the organic layer was washed with saturated saline
  3. customdried
  4. concentrationconcentrated in vacuum
  5. customThe residue was purified by thin-layer silica-gel column chromatography (hexane:ethyl acetate=2:1) and of the title compound (30.7 mg, 92%)
  6. customwas obtained as colorless oil

出典と根拠

ORDレコード
ord-ffd893985cdf44568a5b542a71223e0b
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07951822B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート