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

HRID 329207
ノート
印刷プレビュー

反応式

HRID 329207 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6329MethylamineHCID 12413149HCID 12413149、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-7b860d0adfc641158a5936b340f9b777
出典データセット
uspto-grants-1977_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04020082

反応ノート

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