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Triphenylphosphine → trans-2-(4-Hept-3-enyloxy-phenyl)-5-(5,5,6,6,7,7,8,8,8-nonafluoro-octyloxy)-pyrimidine

HRID 1882751
ノート
印刷プレビュー

反応式

HRID 1882751 の反応式
CCOC(/N=N/C(OCC)=O)=O.[F:13][C:14]([F:43])([C:33]([F:42])([F:41])[C:34]([F:40])([F:39])[C:35]([F:38])([F:37])[F:36])[CH2:15][CH2:16][CH2:17][CH2:18][O:19][C:20]1[CH:21]=[N:22][C:23]([C:26]2[CH:31]=[CH:30][C:29]([OH:32])=[CH:28][CH:27]=2)=[N:24][CH:25]=1.[CH2:44](O)[CH2:45]/[CH:46]=[CH:47]/[CH2:48][CH2:49][CH3:50].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C1COCC1>[CH2:44]([O:32][C:29]1[CH:28]=[CH:27][C:26]([C:23]2[N:22]=[CH:21][C:20]([O:19][CH2:18][CH2:17][CH2:16][CH2:15][C:14]([F:13])([F:43])[C:33]([F:41])([F:42])[C:34]([F:39])([F:40])[C:35]([F:36])([F:37])[F:38])=[CH:25][N:24]=2)=[CH:31][CH:30]=1)[CH2:45]/[CH:46]=[CH:47]/[CH2:48][CH2:49][CH3:50]
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 53180183-Hepten-1-ol, (3E)-HCID 5462977Diethyl azodicarboxylateHCID 1355858974-[5-(5,5,6,6,7,7,8,8,8-Nonafluorooctyloxy)-pyrimidin-2-yl]-phenol

生成物 1

HCID 23509150trans-2-(4-Hept-3-enyloxy-phenyl)-5-(5,5,6,6,7,7,8,8,8-nonafluoro-octyloxy)-pyrimidine

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒
2 回

実験手順

A solution of DEAD (0.261 g, 1.50 mol) in THF (20) was added dropwise to a stirred solution of 4-[5-(5,5,6,6,7,7,8,8,8-nonafluorooctyloxy)-pyrimidin-2-yl]-phenol (0.693 g, 1.50 mmol), trans-3-hepten-1-ol (0.171 g, 1.50 mmol) and triphenylphosphine (0.399 g, 1.50 mmol) in THF (30) and the reaction mixture stirred at room temperature for 16 h. The solvent was removed in vacuo and the residues purified by column chromatography [silica gel, eluted with hexane ethyl acetate (4:1)] to yield a colorless solid, which was recrystallized from ethanol.

後処理

  1. customThe solvent was removed in vacuo
  2. customthe residues purified by column chromatography [silica gel, eluted with hexane ethyl acetate (4:1)]
  3. customto yield a colorless solid, which
  4. customwas recrystallized from ethanol

出典と根拠

ORDレコード
ord-8ff2a0bc534d48aab725d0efd3080df0
出典データセット
uspto-grants-2004_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06759101B2

反応ノート

読み込み中…

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