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Triphenylphosphine → HCID 54510683、化合物

HRID 747778
ノート
印刷プレビュー

反応式

HRID 747778 の反応式
[C:1]([O:5][C:6]([NH:8][C@H:9]([CH2:20][CH2:21][CH2:22][OH:23])[C:10]([O:12][CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)=[O:11])=[O:7])([CH3:4])([CH3:3])[CH3:2].[C:24]([C:26]1[CH:27]=[C:28](O)[CH:29]=[CH:30][CH:31]=1)#[N:25].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][C@H:9]([CH2:20][CH2:21][CH2:22][O:23][C:30]1[CH:29]=[CH:28][CH:27]=[C:26]([C:24]#[N:25])[CH:31]=1)[C:10]([O:12][CH2:13][C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1)=[O:11])=[O:7])([CH3:4])([CH3:3])[CH3:2]
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 133943-CyanophenolHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 53858440benzyl N-(tert-butoxycarbonyl)-5-hydroxy-D-norvalinate

生成物 1

HCID 54510683HCID 54510683、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran
溶媒

実験手順

6.77 g (21 mmol) of benzyl 2-(2R)-t-butoxycarbonylamino-5-hydroxypentanoate was dissolved in 105 ml of tetrahydrofuran. 2.74 g (23 mmol) of 3-cyanophenol, 6.6 g (25 mmol) of triphenylphosphine and 10 g (23 mmol) of diethyl azodicarboxylate (40% solution in toluene) were added to the solution, and they were stirred at room temperature for one hour. The solvent was distilled off, and the residue was treated with ethyl acetate as the extractant in an ordinary manner. The solvent was distilled off, and the residue was purified by the silica gel column chromatography to obtain the title compound.

後処理

  1. distillationThe solvent was distilled off
  2. additionthe residue was treated with ethyl acetate as the extractant in an ordinary manner
  3. distillationThe solvent was distilled off
  4. customthe residue was purified by the silica gel column chromatography

出典と根拠

ORDレコード
ord-6917299838a641ee901d8d37343aaa7d
出典データセット
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07396844B1

反応ノート

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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