Triethylamine → Methanesulfonic Acid

HRID 1946

반응식

HRID 1946 반응식
[CH:1]1([C:7]2[C:8]([OH:37])=[CH:9][C:10]([CH3:36])=[C:11]([CH:13]([C:22]3[CH:27]=[C:26]([CH:28]4[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]4)[C:25]([OH:34])=[CH:24][C:23]=3[CH3:35])[C:14]3[CH:19]=[CH:18][C:17]([OH:20])=[C:16]([OH:21])[CH:15]=3)[CH:12]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[CH3:38][S:39](Cl)(=[O:41])=[O:40].C(N(CC)CC)C>O1CCOCC1>[CH:28]1([C:26]2[C:25]([OH:34])=[CH:24][C:23]([CH3:35])=[C:22]([CH:13]([C:11]3[CH:12]=[C:7]([CH:1]4[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]4)[C:8]([OH:37])=[CH:9][C:10]=3[CH3:36])[C:14]3[CH:19]=[CH:18][C:17]([OH:20])=[C:16]([OH:21])[CH:15]=3)[CH:27]=2)[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]1.[CH3:38][S:39]([OH:41])(=[O:20])=[O:40]

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 157892294-[Bis(5-cyclohexyl-4-hydroxy-2-methylphenyl)methyl]benzene-1,2-diol

생성물 2

HCID 6395Methanesulfonic AcidHCID 157892294-[Bis(5-cyclohexyl-4-hydroxy-2-methylphenyl)methyl]benzene-1,2-diol

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

Bis(5 -cyclohexyl-4-hydroxy-2-methylphenyl)-3,4-dihydroxyphenylmethane(1.0 mole), 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 (1,500 g) having triethylamine (500 g) dissolved therein was added dropwise over 40 minutes at a controlled temperature not higher than 35° C. The precipitating salt was separated by filtration and the thus recovered reaction product was washed and dried to yield a mixed ester of bis(5-cyclohexyl-4-hydroxy-2-methylphenyl)-3,4-dihydroxyphenylmethane with naphthoquinone-1,2-diazido-5-sulfonic acid and methanesulfonic acid; the average degree of esterification was 50% for the quinonediazidosulfonate ester and 12% for the methanesulfonate ester.

후처리

  1. dissolutiondissolved
  2. additiontherein was added dropwise over 40 minutes at a controlled temperature not higher than 35° 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-1a28675e5d044056be5059476c8f3ce9
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05728504

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