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

HRID 2406024

반응식

HRID 2406024 반응식
[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

참가 물질

8

반응물 5

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

생성물 1

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

시약·촉매·용매 2

HCID 75056Tetrahexylammonium iodide촉매HCID 92152Silver(II) oxide촉매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-cf6720065eae450ea255bf8545574cdc
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08809304B2

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