Triethylamine → Methanesulfonic Acid

HRID 1947

반응식

HRID 1947 반응식
[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]

참가 물질

6

반응물 3

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

생성물 2

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-cf4091059f4c4259bc4581b2905f26f6
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05728504

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