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Diethylethanolamine → 2-Diethylaminoethyl 2-[4-(4-chlorophenyl)benzyloxy]-3,3,3-trifluoro-2-trifluoromethylpropionate hydrochloride

HRID 973302
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HRID 973302 반응식
[CH2:1]([N:3]([CH2:7][CH3:8])[CH2:4][CH2:5][OH:6])[CH3:2].[Cl:9][C:10]1[CH:15]=[CH:14][C:13]([C:16]2[CH:35]=[CH:34][C:19]([CH2:20][O:21][C:22]([C:30]([F:33])([F:32])[F:31])([C:26]([F:29])([F:28])[F:27])[C:23](Cl)=[O:24])=[CH:18][CH:17]=2)=[CH:12][CH:11]=1>N1C=CC=CC=1>[ClH:9].[Cl:9][C:10]1[CH:15]=[CH:14][C:13]([C:16]2[CH:17]=[CH:18][C:19]([CH2:20][O:21][C:22]([C:26]([F:27])([F:28])[F:29])([C:30]([F:31])([F:32])[F:33])[C:23]([O:6][CH2:5][CH2:4][N:3]([CH2:7][CH3:8])[CH2:1][CH3:2])=[O:24])=[CH:34][CH:35]=2)=[CH:12][CH:11]=1
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참가 물질

4

반응물 2

HCID 7497DiethylethanolamineHCID 203144652-[4-(4-Chlorophenyl)benzyloxy]-3,3,3-trifluoro-2-trifluoromethylpropionyl chloride

생성물 1

HCID 203144772-Diethylaminoethyl 2-[4-(4-chlorophenyl)benzyloxy]-3,3,3-trifluoro-2-trifluoromethylpropionate hydrochloride수율 112.7%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A mixture of 2-diethylaminoethanol (814 mg.) and pyridine (10 ml.) is added at 0° C. to 2-[4-(4-chlorophenyl)benzyloxy]-3,3,3-trifluoro-2-trifluoromethylpropionyl chloride (3.07 g.). The mixture is stirred at room temperature until the acid chloride dissolves, and the solution is stored at 0° C. for 2 days. The mixture is filtered and the filtrate evaporated. The residue is triturated with ether and combined with the solid previously filtered off. The combined solids are crystallised from dioxan-ether to give 2-diethylaminoethyl 2-[4-(4-chlorophenyl)benzyloxy]-3,3,3-trifluoro-2-trifluoromethylpropionate hydrochloride (2.2 g.), m.p. 139°-140° C. (decomposition).

후처리

  1. dissolutiondissolves
  2. filtrationThe mixture is filtered
  3. customthe filtrate evaporated
  4. customThe residue is triturated with ether
  5. filtrationpreviously filtered off
  6. customThe combined solids are crystallised from dioxan-ether

출처 및 근거

ORD 기록
ord-bb8d44ad1d8846f4a4c253f386cc1f4b
출처 데이터셋
uspto-grants-1977_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04055595

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