3-Hydroxybenzaldehyde → HCID 21071449, 화합물

HRID 1371954노트

반응식

HRID 1371954 반응식
[F:1][C:2]([F:19])([CH:16]([F:18])[F:17])[CH2:3][O:4][C:5]1[CH:6]=[C:7]([CH:12]=[CH:13][C:14]=1C)S([O-])(=O)=O.[OH:20][C:21]1C=C(C=CC=1)C=O.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[F:19][C:2]([F:1])([CH:16]([F:17])[F:18])[CH2:3][O:4][C:5]1[CH:6]=[C:7]([CH:12]=[CH:13][CH:14]=1)[CH:21]=[O:20]

참가 물질

5

반응물 3

HCID 1013-HydroxybenzaldehydeHCID 11430Potassium CarbonateHCID 21071450HCID 21071450, 화합물

생성물 1

HCID 21071449HCID 21071449, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
20 °C

실험 절차

Combine 3-(2,2,3,3-tetrafluoropropoxy)tosylate (5.72 g, 17.2 mmol), 3-hydroxybenzaldehyde (2.44 g, 20.0 mmol), dimethylformamide (36 ml) and powdered potassium carbonate (3.03 g) and heat at 110° C. for 10 h. Cool to 20° C. Pass through a bed of aluminium-oxide-90 (57.2 g, 70–230 mesh, grade II–III, Brockmann: Merck # 1.01097) and elute with toluene (120 ml). Wash the eluted organic phase with 1N HCl (36 ml) and then water. Evaporate the organic layer under reduced pressure to give the title compound.

후처리

  1. washPass through a bed of aluminium-oxide-90 (57.2 g, 70–230 mesh, grade II–III, Brockmann: Merck # 1.01097) and elute with toluene (120 ml)
  2. washWash the eluted organic phase with 1N HCl (36 ml)
  3. customEvaporate the organic layer under reduced pressure

출처 및 근거

ORD 기록
ord-d20678c3df594e1597028407b2f52ed1
출처 데이터셋
uspto-grants-2007_01
특허 번호
US07157488B2

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