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Sodium → 2,6-Bis(trifluoromethyl)benzenemethanol

HRID 1720085
ノート
印刷プレビュー

反応式

HRID 1720085 の反応式
[H-].C([Al+]CC(C)C)C(C)C.[F:11][C:12]([F:28])([F:27])[C:13]1[CH:22]=[CH:21][CH:20]=[C:19]([C:23]([F:26])([F:25])[F:24])[C:14]=1[C:15](OC)=[O:16].[K].[Na]>C1(C)C=CC=CC=1>[F:11][C:12]([F:27])([F:28])[C:13]1[CH:22]=[CH:21][CH:20]=[C:19]([C:23]([F:26])([F:24])[F:25])[C:14]=1[CH2:15][OH:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 5360545SodiumHCID 5462222PotassiumHCID 21225700DiisobutylaluminumhydrideHCID 22420073Methyl 2,6-bis(trifluoromethyl)benzoate

生成物 1

HCID 153464312,6-Bis(trifluoromethyl)benzenemethanol収率 94.1%

試薬・触媒・溶媒 1

HCID 1140Toluene
溶媒

実験手順

58 ml of a 1.2M solution of diisobutylaluminium hydride (DIBAH) were added at 0° C. to a solution of 5.59 g of the product of Stage A and 60 ml of toluene. The temperature was allowed to return to 20° C. and the reaction mixture was stirred for 4 hours, then poured into a molar solution of potassium and sodium double tartrate and extracted with isopropyl ether. The aqueous phase was saturated with sodium chloride, followed by extraction with ethyl acetate, drying, filtering, rinsing and bringing to dryness to obtain after chromatography on silica (eluant: hexane-ethyl acetate (9-1)), 4.72 g of the desired product.

後処理

  1. customto return to 20° C.
  2. extractionextracted with isopropyl ether
  3. extractionfollowed by extraction with ethyl acetate
  4. customdrying
  5. filtrationfiltering
  6. washrinsing

出典と根拠

ORDレコード
ord-85784df3dd1b437eb489df32cab2f0c6
出典データセット
uspto-grants-1996_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05504112

反応ノート

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