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Sodium → 2,6-Bis(trifluoromethyl)benzenemethanol

HRID 1720085
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인쇄 미리보기

반응식

HRID 1720085 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

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

생성물 1

HCID 153464312,6-Bis(trifluoromethyl)benzenemethanol수율 94.1%

시약·촉매·용매 1

HCID 1140Toluene
용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-85784df3dd1b437eb489df32cab2f0c6
출처 데이터셋
uspto-grants-1996_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05504112

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