(2-(4-Bromophenoxy)ethyl)dimethylamine → HCID 20216187, 화합물

HRID 236562

반응식

HRID 236562 반응식
[Mg].[CH3:2][N:3]([CH3:14])[CH2:4][CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10](Br)=[CH:9][CH:8]=1.[Cl:15][C:16]1[CH:17]=[C:18]([C:22](=[O:25])[CH2:23][CH3:24])[CH:19]=[CH:20][CH:21]=1>O1CCCC1>[CH2:23]([C:22]([OH:25])([C:18]1[CH:19]=[CH:20][CH:21]=[C:16]([Cl:15])[CH:17]=1)[C:10]1[CH:11]=[CH:12][C:7]([O:6][CH2:5][CH2:4][N:3]([CH3:14])[CH3:2])=[CH:8][CH:9]=1)[CH3:24]

참가 물질

5

반응물 3

HCID 213877(2-(4-Bromophenoxy)ethyl)dimethylamineHCID 5871283'-ChloropropiophenoneHCID 5462224Magnesium

생성물 1

HCID 20216187HCID 20216187, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a Grignard reactant prepared from 2.2 g. of magnesium turnings and 23.4 g. of 4-[2-(dimethylamino)-ethoxy]-bromobenzene in 100 ml. of dry tetrahydrofurane a solution of 10 g. of m-chloro-propiophenone in 30 ml. of tetrahydrofurane is added dropwise, at 20° C. The reaction mixture is stirred at room temperature for another two hours, cooled, and filtered onto a 20% aqueous ammonium chloride solution. Tetrahydrofurane is distilled off in vacuo. The residue is extracted with ether, the ethereal phase is washed with water, dried over anhydrous magnesium sulfate, filtered, and ether is distilled off. Crystallization of the residue from a mixture of n-hexane and ethyl acetate yields 14.2 g. of the named compound, melting at 108° to 109° C.

후처리

  1. temperaturecooled
  2. filtrationfiltered onto a 20% aqueous ammonium chloride solution
  3. distillationTetrahydrofurane is distilled off in vacuo
  4. extractionThe residue is extracted with ether
  5. washthe ethereal phase is washed with water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. filtrationfiltered
  8. distillationether is distilled off
  9. customCrystallization of the residue
  10. additionfrom a mixture of n-hexane and ethyl acetate
  11. customyields 14.2 g

출처 및 근거

ORD 기록
ord-f166782117584096ac805d8aeac5b5c5
출처 데이터셋
uspto-grants-1987_02
특허 번호
US04645774

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