Morpholine → HCID 13690981、化合物

HRID 2290781ノート

反応式

HRID 2290781 の反応式
Cl[CH2:2][C:3]1[N:7]=[C:6]([CH:8]([CH3:22])[C:9]2[CH:14]=[CH:13][C:12]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)=[C:11]([F:21])[CH:10]=2)[O:5][N:4]=1.[NH:23]1[CH2:28][CH2:27][O:26][CH2:25][CH2:24]1>CN(C=O)C>[F:21][C:11]1[CH:10]=[C:9]([CH:14]=[CH:13][C:12]=1[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[CH:8]([C:6]1[O:5][N:4]=[C:3]([CH2:2][N:23]2[CH2:28][CH2:27][O:26][CH2:25][CH2:24]2)[N:7]=1)[CH3:22]

参加物

4

反応物 2

HCID 8083MorpholineHCID 136909413-Chloromethyl-5-(3-fluoro-4-phenyl-alpha-methylbenzyl)-1,2,4-oxadiazole

生成物 1

HCID 13690981HCID 13690981、化合物収率 103.8%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 1.52 g of 3-chloromethyl-5-(3-fluoro-4-phenyl-α-methylbenzyl)-1,2,4-oxadiazole in 30 ml of DMF was added 1.68 g of morpholine. The mixture was allowed to stand at room temperature overnight, then poured into ice-water and extracted with benzene. The organic phase was washed with water, dried over sodium sulfate and evaporated. The residue was chromatographed over silica gel using benzene-ethyl acetate (5:2, v/v) as an eluent to yield 1.83 g of 5-(3-fluoro-4-phenyl-α-methylbenzyl)-3-morpholinomethyl-1,2,4-oxadiazole as an oil. It was crystallized from diisopropyl ether to give colorless needles, m.p. 91.5°-92.5° C.

後処理

  1. extractionextracted with benzene
  2. washThe organic phase was washed with water
  3. dry with materialdried over sodium sulfate
  4. customevaporated
  5. customThe residue was chromatographed over silica gel

出典と根拠

ORDレコード
ord-feda91d9402e4e5db25af51d6422b52e
出典データセット
uspto-grants-1986_10
特許番号
US04618617

反応ノート

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