反応 #2043

ord-cf4091059f4c4259bc4581b2905f26f6

反応方程式

CC(C)(c1ccc(O)cc1)c1ccc(C(C)(c2ccc(O)cc2)c2ccc(O)cc2)cc1
1-[1-(4-hydroxyphenyl)isopropyl]-4-[1,1-bis(4-hydroxyphenyl)ethyl]benzene
CS(=O)(=O)Cl
methanesulfonyl chloride
CCN(CC)CC
triethylamine
CC(C)(c1ccc(O)cc1)c1ccc(C(C)(c2ccc(O)cc2)c2ccc(O)cc2)cc1
1-[1-(4-hydroxyphenyl)isopropyl]-4-[1,1-bis(4-hydroxyphenyl)ethyl]benzene
CS(=O)(=O)O
methanesulfonic acid

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.DISSOLUTIONdissolved
  2. 2
    workup.ADDITIONtherein was added dropwise over 10 minutes at a controlled temperature not higher than 30° C
  3. 3
    その他The precipitating salt was separated by filtration
  4. 4
    その他the thus recovered reaction product
  5. 5
    洗浄was washed
  6. 6
    その他dried

実験手順

One (1.0) mole of 1-[1-(4-hydroxyphenyl)isopropyl]-4-[1,1-bis(4-hydroxyphenyl)ethyl]benzene, naphthoquinone-1,2-diazido-5-sulfonyl chloride (2.0 moles) and methanesulfonyl chloride (0.5 moles) were dissolved in dioxane (4,000 g). To the resulting solution, dioxane (2,000 g) having triethylamine (500 g) dissolved therein was added dropwise over 10 minutes at a controlled temperature not higher than 30° C. The precipitating salt was separated by filtration and the thus recovered reaction product was washed and dried to yield esters of the 1-[1-(4-hydroxyphenyl)isopropyl]-4-[1,1-bis(4-hydroxyphenyl)ethyl]benzene with naphthoquinone-1,2-diazido-5-sulfonic acid and methanesulfonic acid.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05728504uspto-grants-1998_03