Triphenylphosphine → 2-[4-[(5E)-5-Decen-1-yloxy]phenyl]-5-[(5,5,6,6,7,7,8,8,8-nonafluorooctyl)oxy]pyrimidine

HRID 1882750

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][CH2:46][CH2:47]/[CH:48]=[CH:49]/[CH2:50][CH2:51][CH2:52][CH3:53].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][CH2:46][CH2:47]/[CH:48]=[CH:49]/[CH2:50][CH2:51][CH2:52][CH3:53]

参加物

実験手順

A solution of DEAD (0.261 g, 1.50 mmol) 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-5-decen-1-ol (0.234 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

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

出典と根拠

ORDレコード: ord-104789d05eba48a690decbce1e4e773a
出典データセット: uspto-grants-2004_07
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US06759101B2

反応式

参加物

反応物 4

生成物 1

試薬・触媒・溶媒 1

実験手順

後処理

出典と根拠

関連ノート