Tetrahydrofuran → 3-(5-Methyl-2-phenyl-4-oxazolylmethoxy)benzyloxyamine

HRID 1070060

反応式

HRID 1070060 の反応式
O.NN.[CH3:4][C:5]1[O:9][C:8]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[N:7][C:6]=1[CH2:16][O:17][C:18]1[CH:19]=[C:20]([CH:34]=[CH:35][CH:36]=1)[CH2:21][O:22][N:23]1C(=O)C2=CC=CC=C2C1=O.O1CCCC1.C(=O)([O-])[O-].[K+].[K+]>C(O)C>[CH3:4][C:5]1[O:9][C:8]([C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=2)=[N:7][C:6]=1[CH2:16][O:17][C:18]1[CH:19]=[C:20]([CH:34]=[CH:35][CH:36]=1)[CH2:21][O:22][NH2:23]

参加物

6

反応物 4

HCID 8028TetrahydrofuranHCID 11430Potassium CarbonateHCID 24654Hydrazine hydrate (1:1)HCID 11732904N-[3-(5-methyl-2-phenyl-4-oxazolylmethoxy)benzyloxy]phthalimide

生成物 1

HCID 109249463-(5-Methyl-2-phenyl-4-oxazolylmethoxy)benzyloxyamine収率 97%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Hydrazine monohydrate (0.661 ml) was added to a solution of N-[3-(5-methyl-2-phenyl-4-oxazolylmethoxy)benzyloxy]phthalimide (3.00 g) in ethanol (25 ml)-tetrahydrofuran (25 ml) and heated under reflux for 3 hours. The reaction mixture was cooled to room temperature, an aqueous solution of potassium carbonate was added and extracted with ethyl acetate. The ethyl acetate layer was washed with an aqueous saturated solution of sodium chloride, dried (MgSO4) and concentrated. The remaining crystals were recrystallized from ethyl acetate-hexane to obtain 3-(5-methyl-2-phenyl-4-oxazolylmethoxy)benzyloxyamine (2.04 g, yield 97%) as pale-yellow crystals. m.p. 81-82° C.

後処理

  1. temperatureheated
  2. temperatureunder reflux for 3 hours
  3. extractionextracted with ethyl acetate
  4. washThe ethyl acetate layer was washed with an aqueous saturated solution of sodium chloride
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated
  7. customThe remaining crystals were recrystallized from ethyl acetate-hexane

出典と根拠

ORDレコード
ord-9cd42e1797b740298216b5ddeb00115d
出典データセット
uspto-grants-2001_06
特許番号
US06251926B1

関連ノート

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