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Acetic Acid → HCID 22344564、化合物

HRID 584456
ノート
印刷プレビュー

反応式

HRID 584456 の反応式
[CH3:1][C:2]1[O:6][C:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)=[N:4][C:3]=1[CH2:13][O:14][C:15]1[CH:23]=[CH:22][C:18]([CH2:19][O:20][NH2:21])=[CH:17][CH:16]=1.[O:24]1[CH:28]=[CH:27][CH:26]=[C:25]1[C:29](=O)[CH2:30][CH2:31][C:32]([O:34][CH2:35][CH3:36])=[O:33].C(O)(=O)C.C([O-])(=O)C.[Na+]>C(OCC)(=O)C.CCCCCC.O.C(O)C>[O:24]1[CH:28]=[CH:27][CH:26]=[C:25]1/[C:29](=[N:21]/[O:20][CH2:19][C:18]1[CH:17]=[CH:16][C:15]([O:14][CH2:13][C:3]2[N:4]=[C:5]([C:7]3[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=3)[O:6][C:2]=2[CH3:1])=[CH:23][CH:22]=1)/[CH2:30][CH2:31][C:32]([O:34][CH2:35][CH3:36])=[O:33]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 176Acetic AcidHCID 517045Sodium AcetateHCID 9990260HCID 9990260、化合物HCID 223445934-(5-Methyl-2-phenyl4-oxazolylmethoxy)benzyloxyamine

生成物 1

HCID 22344564HCID 22344564、化合物収率 24.1%

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒
HCID 962Water溶媒
HCID 21226206Ethyl acetate hexane溶媒

実験手順

After a mixture of 4-(5-methyl-2-phenyl-4-oxazolylmethoxy)benzyloxyamine (500 mg), ethyl 4-(2-furyl)-4-oxobutyrate (347 mg), acetic acid (0.276 ml), sodium acetate (264 mg) and ethanol (20 ml) was heated to reflux for 96 hours, the mixture was cooled to room temperature. Water was added to the reaction mixture and extracted with ethyl acetate. The ethyl acetate layer was washed with an aqueous saturated solution of sodium chloride, dried (MgSO4) and concentrated. The residue was subjected to silica gel chromatography to obtain ethyl E-4-(2-furyl)-4-[4-(5-methyl-2-phenyl-4-oxazolylmethoxy)benzyloxyimino]butyrate (190 mg, yield 24%) as a colorless oil from an ethyl acetate-hexane (1:4, v/v)-eluted fraction.

後処理

  1. temperaturewas heated
  2. temperatureto reflux for 96 hours
  3. extractionextracted with ethyl acetate
  4. washThe ethyl acetate layer was washed with an aqueous saturated solution of sodium chloride
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-07d856aee4314563a41757f11c743061
出典データセット
uspto-grants-2005_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06924300B2

反応ノート

読み込み中…

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