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Methylamine → Oxazole, 4,5-diphenyl-2-((methylamino)methyl)-, monohydrochloride

HRID 329207
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HRID 329207 반응식
[Cl:1][CH2:2][C:3]1[O:4][C:5]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[N:7]=1.[CH3:20][NH2:21]>C1C=CC=CC=1>[ClH:1].[CH3:20][NH:21][CH2:2][C:3]1[O:4][C:5]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[N:7]=1
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참가 물질

4

반응물 2

HCID 6329MethylamineHCID 12413149HCID 12413149, 화합물

생성물 1

HCID 214399Oxazole, 4,5-diphenyl-2-((methylamino)methyl)-, monohydrochloride수율 69%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

A solution of 22 g. 2-chloromethyl-4,5-diphenyloxazole and 12.5 g methylamine in 100 ml. anhydrous benzene was heated at 120° C for 6 hours in a sealed tube. The reaction mixture was washed with water and the separated benzene phase was distilled at 20 mm. pressure. The oily residue was dissolved in 200 ml. anhydrous ether and a flow of gas hydrogen chloride was bubbled through the resulting solution. The 2-methylaminomethyl-4,5-diphenyloxazole hydrochloride was recrystallized from absolute ethanol: 16.5 g., m.p. 207°-208° C (yield 69%).

후처리

  1. washThe reaction mixture was washed with water
  2. distillationthe separated benzene phase was distilled at 20 mm
  3. dissolutionThe oily residue was dissolved in 200 ml
  4. customanhydrous ether and a flow of gas hydrogen chloride was bubbled through the resulting solution
  5. customThe 2-methylaminomethyl-4,5-diphenyloxazole hydrochloride was recrystallized from absolute ethanol

출처 및 근거

ORD 기록
ord-7b860d0adfc641158a5936b340f9b777
출처 데이터셋
uspto-grants-1977_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04020082

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