Toluene → [1-(dibenzyl)phosphoryloxymethyl-1-hydroxymethyl-3-(4-heptyloxy-3-trifluoromethylphenyl)propyl]carbamic Acid Benzyl Ester

HRID 2406024

反応式

HRID 2406024 の反応式
[CH2:1]([O:8][C:9](=[O:36])[NH:10][C:11]([CH2:34][OH:35])([CH2:32][OH:33])[CH2:12][CH2:13][C:14]1[CH:19]=[CH:18][C:17]([O:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27])=[C:16]([C:28]([F:31])([F:30])[F:29])[CH:15]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C([O:44][P:45](OP(OCC1C=CC=CC=1)(OCC1C=CC=CC=1)=O)(OCC1C=CC=CC=1)=O)C1C=CC=CC=1.[C:74]1([CH3:80])[CH:79]=[CH:78][CH:77]=[CH:76][CH:75]=1.F[C:82](F)(F)[C:83](F)(F)[C:84](F)(F)[C:85](F)(F)[C:86](F)(F)[C:87](F)(F)F.Cl[CH2:102]Cl>[I-].C([N+](CCCCCC)(CCCCCC)CCCCCC)CCCCC.[Ag]=O>[CH2:1]([O:8][C:9](=[O:36])[NH:10][C:11]([CH2:34][O:35][P:45]([CH2:82][C:83]1[CH:102]=[CH:87][CH:86]=[CH:85][CH:84]=1)([CH2:80][C:74]1[CH:79]=[CH:78][CH:77]=[CH:76][CH:75]=1)=[O:44])([CH2:32][OH:33])[CH2:12][CH2:13][C:14]1[CH:19]=[CH:18][C:17]([O:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27])=[C:16]([C:28]([F:31])([F:30])[F:29])[CH:15]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

8

反応物 5

HCID 1140TolueneHCID 6344DichloromethaneHCID 9639PerfluorohexaneHCID 563183Tetrabenzyl pyrophosphateHCID 57704545[1,1-bis(hydroxymethyl)-3-(4-heptyloxy-3-trifluoromethylphenyl)propyl]carbamic Acid Benzyl Ester

生成物 1

HCID 67417982[1-(dibenzyl)phosphoryloxymethyl-1-hydroxymethyl-3-(4-heptyloxy-3-trifluoromethylphenyl)propyl]carbamic Acid Benzyl Ester

試薬・触媒・溶媒 2

HCID 75056Tetrahexylammonium iodide触媒HCID 92152Silver(II) oxide触媒

実験手順

Compound 2-1 (230 mg), pyrophosphoric acid tetrabenzyl ester (485 mg), silver oxide (208 mg) and tetra-n-hexyl ammonium iodide (433 mg) were added to a mixed solvent of toluene (4 ml), dichloromethane (4 ml) and perfluorohexane (4 ml), and the mixture was stirred at room temperature for 15 hr. Insoluble material was filtered off and the solvent was evaporated under reduced pressure. The residue was purified by preparative HPLC to give the object product (210 mg) as a colorless oil.

後処理

  1. filtrationInsoluble material was filtered off
  2. customthe solvent was evaporated under reduced pressure
  3. customThe residue was purified by preparative HPLC

出典と根拠

ORDレコード
ord-cf6720065eae450ea255bf8545574cdc
出典データセット
uspto-grants-2014_08
特許番号
US08809304B2

関連ノート

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