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Hydrochloric Acid → 2,2-Bis-(4-mesyloxy-3-nitrophenyl)-hexafluoropropane

HRID 1086324
ノート
印刷プレビュー

反応式

HRID 1086324 の反応式
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[OH:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]([C:22]2[CH:27]=[CH:26][C:25]([OH:28])=[C:24]([N+:29]([O-:31])=[O:30])[CH:23]=2)([C:18]([F:21])([F:20])[F:19])[C:14]([F:17])([F:16])[F:15])=[CH:9][C:8]=1[N+:32]([O-:34])=[O:33].Cl>N1C=CC=CC=1>[S:2]([O:28][C:25]1[CH:26]=[CH:27][C:22]([C:13]([C:10]2[CH:11]=[CH:12][C:7]([O:6][S:2]([CH3:1])(=[O:4])=[O:3])=[C:8]([N+:32]([O-:34])=[O:33])[CH:9]=2)([C:18]([F:21])([F:19])[F:20])[C:14]([F:16])([F:15])[F:17])=[CH:23][C:24]=1[N+:29]([O-:31])=[O:30])([CH3:1])(=[O:4])=[O:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 31297Methanesulfonyl chlorideHCID 111336832,2-Bis(3-nitro-4-hydroxyphenyl)hexafluoropropane

生成物 1

HCID 142050422,2-Bis-(4-mesyloxy-3-nitrophenyl)-hexafluoropropane収率 85%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

11.5 g (0.1 mol) of methanesulfonyl chloride are added dropwise, at a reaction temperature of 0-5° C., to a mixture of 21.3 g (0.05 mol) of 2,2-bis-(4-hydroxy-3-nitrophenyl)-hexafluoropropane and 100 ml of pyridine. Stirring is continued for 1 hour at 5° C. and overnight at room temperature. The reaction mixture is then acidified, first with dilute hydrochloric and then with half-concentrated hydrochloric acid; the precipitate which is deposited is filtered off with suction and washed with water until neutral. The crude product (29.3 g) is then recrystallized from toluene, resulting in 24.8 g of analytically pure 2,2-bis-(4-mesyloxy-3-nitrophenyl)-hexafluoropropane to be isolated. Yield 85%; m.p. 119-121° C.

後処理

  1. additionfirst with dilute hydrochloric
  2. filtrationthe precipitate which is deposited is filtered off with suction
  3. washwashed with water until neutral
  4. customThe crude product (29.3 g) is then recrystallized from toluene

出典と根拠

ORDレコード
ord-367d7b325d334add9a422dc99a56328d
出典データセット
uspto-grants-1991_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05028728

反応ノート

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