Water → 1,3,5-Trimethyl-2,4-bis-(2,2,2-trifluoro-1-p-tolyl-1-trifluoromethylethoxy-sulfonyl)-benzene

HRID 861844

反応式

HRID 861844 の反応式
[F:1][C:2]([F:17])([F:16])[C:3]([C:9]1[CH:14]=[CH:13][C:12]([CH3:15])=[CH:11][CH:10]=1)([OH:8])[C:4]([F:7])([F:6])[F:5].[H-].[Na+].[CH3:20][C:21]1[C:26]([S:27](Cl)(=[O:29])=[O:28])=[C:25]([CH3:31])[CH:24]=[C:23]([CH3:32])[C:22]=1[S:33](Cl)(=[O:35])=[O:34].[OH2:37]>CN(C=O)C>[CH3:32][C:23]1[CH:24]=[C:25]([CH3:31])[C:26]([S:27]([O:8][C:3]([C:4]([F:6])([F:5])[F:7])([C:9]2[CH:14]=[CH:13][C:12]([CH3:15])=[CH:11][CH:10]=2)[C:2]([F:16])([F:17])[F:1])(=[O:29])=[O:28])=[C:21]([CH3:20])[C:22]=1[S:33]([O:35][C:3]([C:9]1[CH:10]=[CH:11][C:12]([CH3:15])=[CH:13][CH:14]=1)([C:2]([F:17])([F:1])[F:16])[C:4]([F:7])([F:6])[F:5])(=[O:37])=[O:34]

参加物

6

反応物 4

HCID 962WaterHCID 24758Sodium hydrideHCID 748292-(p-Tolyl)hexafluoroisopropanolHCID 36200812,4-Mesitylenedisulfonyl Dichloride

生成物 1

HCID 197002851,3,5-Trimethyl-2,4-bis-(2,2,2-trifluoro-1-p-tolyl-1-trifluoromethylethoxy-sulfonyl)-benzene

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

7.75 g (30 mmol) of 1,1,1,3,3,3-hexafluoro-2-p-tolylpropan-2-ol were dissolved in 45 ml of DMF, and 1.2 g (40 mmol) of NaH (80% strength dispersion in mineral oil) were added. After a clear solution had formed, 5.0 g (14 mmol) of 2,4,6-trimethylbenzene-1,3-disulfonyl chloride were added and the mixture was stirred for a further 72 hours at room temperature. The mixture was poured into water and the precipitated product was filtered off and dried. 7.8 g of 1,3,5-trimethyl-2,4-bis-(2,2,2-trifluoro-1-p-tolyl-1-trifluoromethylethoxy-sulfonyl)-benzene were obtained (colorless crystals, m.p.: 178° C. [from acetonitrile]).

後処理

  1. customAfter a clear solution had formed
  2. filtrationthe precipitated product was filtered off
  3. customdried

出典と根拠

ORDレコード
ord-b66eebdf74734621acbce13e2060fdb5
出典データセット
uspto-grants-1998_02
特許番号
US05716756

関連ノート

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