Triethylamine → Methanesulfonic Acid

HRID 1947

反応式

HRID 1947 の反応式
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:11]2[CH:16]=[CH:15][C:14]([C:17]([C:26]3[CH:31]=[CH:30][C:29]([OH:32])=[CH:28][CH:27]=3)([C:19]3[CH:24]=[CH:23][C:22]([OH:25])=[CH:21][CH:20]=3)[CH3:18])=[CH:13][CH:12]=2)([CH3:10])[CH3:9])=[CH:4][CH:3]=1.[CH3:33][S:34](Cl)(=[O:36])=[O:35].C(N(CC)CC)C>O1CCOCC1>[OH:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:11]2[CH:16]=[CH:15][C:14]([C:17]([C:19]3[CH:20]=[CH:21][C:22]([OH:25])=[CH:23][CH:24]=3)([C:26]3[CH:31]=[CH:30][C:29]([OH:32])=[CH:28][CH:27]=3)[CH3:18])=[CH:13][CH:12]=2)([CH3:10])[CH3:9])=[CH:4][CH:3]=1.[CH3:33][S:34]([OH:36])(=[O:1])=[O:35]

参加物

6

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 6342784,4'-(1-(4-(1-(4-Hydroxyphenyl)-1-methylethyl)phenyl)ethylidene)diphenol

生成物 2

HCID 6395Methanesulfonic AcidHCID 6342784,4'-(1-(4-(1-(4-Hydroxyphenyl)-1-methylethyl)phenyl)ethylidene)diphenol

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

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.

後処理

  1. dissolutiondissolved
  2. additiontherein was added dropwise over 10 minutes at a controlled temperature not higher than 30° C
  3. customThe precipitating salt was separated by filtration
  4. customthe thus recovered reaction product
  5. washwas washed
  6. customdried

出典と根拠

ORDレコード
ord-cf4091059f4c4259bc4581b2905f26f6
出典データセット
uspto-grants-1998_03
特許番号
US05728504

関連ノート

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