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Triphenylphosphine → 3-[2-Tert-butoxycarbonylamino-3-(3-benzenesulfonyloxy-5-isoxazolyl)propoxy]-5-chloro-1,2-benzoisoxazole

HRID 1901645
ノート
印刷プレビュー

反応式

HRID 1901645 の反応式
[C:1]([O:5][C:6]([NH:8][CH:9]([CH2:12][C:13]1[O:17][N:16]=[C:15]([O:18][S:19]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)(=[O:21])=[O:20])[CH:14]=1)[CH2:10][OH:11])=[O:7])([CH3:4])([CH3:3])[CH3:2].[Cl:28][C:29]1[CH:30]=[CH:31][C:32]2[O:36][N:35]=[C:34](O)[C:33]=2[CH:38]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OCC)=O)=NC(OCC)=O>O1CCCC1>[C:1]([O:5][C:6]([NH:8][CH:9]([CH2:12][C:13]1[O:17][N:16]=[C:15]([O:18][S:19]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)(=[O:20])=[O:21])[CH:14]=1)[CH2:10][O:11][C:34]1[C:33]2[CH:38]=[C:29]([Cl:28])[CH:30]=[CH:31][C:32]=2[O:36][N:35]=1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
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 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 233684952-Tert-butoxycarbonylamino-3-(3-benzenesulfonyloxyisoxazol-5-yl)-1-propanolHCID 178518984HCID 178518984、化合物

生成物 1

HCID 233684903-[2-Tert-butoxycarbonylamino-3-(3-benzenesulfonyloxy-5-isoxazolyl)propoxy]-5-chloro-1,2-benzoisoxazole収率 73.4%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 0.5 g of 2-tert-butoxycarbonylamino-3-(3-benzenesulfonyloxyisoxazol-5-yl)-1-propanol in 5 ml of tetrahydrofuran are added 0.21 g of 5-chloro-3-hydroxy-1,2-benzoisoxazole, 0.43 g of triphenylphosphine and 0.28 g of diethyl azodicarboxylate with ice-cooling, and they are subjected to reaction at room temperature for 24 hours. Thereafter, the solvent is removed by distillation under reduced pressure. The residue obtained is purified by a column chromatography [eluant:n-hexane:ethyl acetate=4:1], to obtain 0.5 g of oily 3-[2-tert-butoxycarbonylamino-3-(3-benzenesulfonyloxy-5-isoxazolyl)propoxy]-5-chloro-1,2-benzoisoxazole.

後処理

  1. temperaturecooling
  2. customthey are subjected to reaction at room temperature for 24 hours
  3. customThereafter, the solvent is removed by distillation under reduced pressure
  4. customThe residue obtained
  5. customis purified by a column chromatography [eluant:n-hexane:ethyl acetate=4:1]

出典と根拠

ORDレコード
ord-05123b0f23e243eabd95df5d2c350898
出典データセット
uspto-grants-1996_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05578627

反応ノート

読み込み中…

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