Triethylamine → Methanesulfonic Acid

HRID 1946

反応式

HRID 1946 の反応式
[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]

参加物

6

反応物 3

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

生成物 2

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

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1a28675e5d044056be5059476c8f3ce9
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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