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Water → HCID 11591698、化合物

HRID 2076601
ノート
印刷プレビュー

反応式

HRID 2076601 の反応式
N1CCOCC1.C([O:10][C:11]1[C:23]([C:24]([F:27])([F:26])[F:25])=[CH:22][CH:21]=[C:20]([CH2:28][O:29][C:30]2[CH:35]=[CH:34][C:33]([C:36]3[CH:41]=[CH:40][C:39]([CH2:42][C:43]([O:45]CC=C)=[O:44])=[C:38]([F:49])[CH:37]=3)=[CH:32][CH:31]=2)[C:12]=1[C:13]([O:15][C:16]([CH3:19])([CH3:18])[CH3:17])=[O:14])C=C.O>O1CCCC1.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[C:16]([O:15][C:13]([C:12]1[C:11]([OH:10])=[C:23]([C:24]([F:27])([F:25])[F:26])[CH:22]=[CH:21][C:20]=1[CH2:28][O:29][C:30]1[CH:31]=[CH:32][C:33]([C:36]2[CH:41]=[CH:40][C:39]([CH2:42][C:43]([OH:45])=[O:44])=[C:38]([F:49])[CH:37]=2)=[CH:34][CH:35]=1)=[O:14])([CH3:19])([CH3:17])[CH3:18]
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 3

HCID 962WaterHCID 8083MorpholineHCID 67119033HCID 67119033、化合物

生成物 1

HCID 11591698HCID 11591698、化合物収率 47%

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒HCID 8028Tetrahydrofuran
溶媒

実験手順

Morpholine (0.27 ml, 3.3 mmol) and tetrakis(triphenylphosphine)palladium (0) (57 mg, 0.049 mmol) were successively added to a solution of tert-butyl 2-(allyloxy)-6-{[(4′-{[(allyloxy)carbonyl]methyl}-3′-fluoro-1,1′-biphenyl-4-yl)oxy]methyl}-3-(trifluoromethyl)benzoate (790 mg, 1.32 mmol) obtained in Example (11-6) in tetrahydrofuran (8 ml), and the mixture was stirred at room temperature for 1 hour. After water was poured into the reaction mixture and the mixture was extracted with ethyl acetate, the organic layer was successively washed with water and a saturated aqueous NaCl solution and dried with anhydrous sodium sulfate. After the residue obtained by removing the solvent under reduced pressure was purified by silica gel column chromatography (eluting solvent: n-hexane/ethyl acetate=3/1-0/1), it was crystallized from a mixture solvent of methylene chloride-ethyl acetate to give the title compound as a colorless powder (323 mg, yield: 47%).

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washthe organic layer was successively washed with water
  3. dry with materiala saturated aqueous NaCl solution and dried with anhydrous sodium sulfate
  4. customAfter the residue obtained
  5. customby removing the solvent under reduced pressure
  6. customwas purified by silica gel column chromatography (eluting solvent: n-hexane/ethyl acetate=3/1-0/1), it
  7. customwas crystallized from a mixture solvent of methylene chloride-ethyl acetate

出典と根拠

ORDレコード
ord-ed32fbd9a7a54ceeb0d2229050f364fb
出典データセット
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07923573B2

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