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N-isobutylidene-3-phenoxybenzylamine → 3-Phenoxybenzylidene-isobutylamine

HRID 224269
ノート
印刷プレビュー

反応式

HRID 224269 の反応式
[CH:1](=[N:5][CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([O:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH:8]=1)[CH:2]([CH3:4])[CH3:3]>CS(C)=O>[O:13]([C:9]1[CH:8]=[C:7]([CH:12]=[CH:11][CH:10]=1)[CH:6]=[N:5][CH2:1][CH:2]([CH3:3])[CH3:4])[C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 23332476N-isobutylidene-3-phenoxybenzylamine

生成物 1

HCID 233324743-Phenoxybenzylidene-isobutylamine収率 95%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

51 g (0.202 mol) of N-isobutylidene-(3-phenoxybenzylamine) is dissolved in 45 ml of dimethyl sulfoxide, and at room temperature (20°-25° C.) is added all at once, with stirring, 2 g (0.0179 mol) of potassium-tert-butylate. The temperature of the reaction solution rises during this addition to 25°-30° C. The solution is stirred for a further hour at room temperature, and is then extracted three times with 50 ml of water each time. The residue is taken up in 30 ml of diethyl ether, dried with magnesium sulfate, and distilled to obtain 48.5 g (0.192 mol) of 3-phenoxybenzylidene-isobutylamine, corresponding to a yield of 95% of theory; b.p. 83° C./4 Pa; nD20 =1.5677.

後処理

  1. additionat room temperature (20°-25° C.) is added all at once,
  2. additionThe temperature of the reaction solution rises during this addition to 25°-30° C
  3. stirringThe solution is stirred for a further hour at room temperature
  4. extractionis then extracted three times with 50 ml of water each time
  5. dry with materialdried with magnesium sulfate
  6. distillationdistilled

出典と根拠

ORDレコード
ord-bc88634d1d5d44a0888471f6fa72b2d6
出典データセット
uspto-grants-1980_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04231962

反応ノート

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