Water → N-isobutylidene-3-phenoxybenzylamine

HRID 224268ノート

反応式

HRID 224268 の反応式
[CH:1](=O)[CH:2]([CH3:4])[CH3:3].[O:6]([C:13]1[CH:14]=[C:15]([CH:18]=[CH:19][CH:20]=1)[CH2:16][NH2:17])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.O>C1(C)C=CC=CC=1>[CH:1](=[N:17][CH2:16][C:15]1[CH:18]=[CH:19][CH:20]=[C:13]([O:6][C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH:14]=1)[CH:2]([CH3:4])[CH3:3]

参加物

5

反応物 3

HCID 962WaterHCID 6561IsobutyraldehydeHCID 10948363-Phenoxy-benzylamine

生成物 1

HCID 23332476N-isobutylidene-3-phenoxybenzylamine収率 98%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

38 g (0.528 mol) of isobutyraldehyde is added dropwise within 30 minutes, with stirring, to a solution of 99.5 g (0.5 mol) of 3-phenoxybenzylamine in 100 ml of toluene. After completion of the dropwise addition, stirring is continued for 20 minutes at room temperature, and the water which has formed (about 8.5 g) is separated in a separating funnel. The toluene with the unreacted isobutyraldehyde and residual water is then removed by rotation in a water-jet vacuum, and the residue is distilled in an oil-pump vacuum to yield 124 g (0.49 mol) of N-isobutylidene-(3-phenoxybenzylamine) as a colourless, mobile liquid, corresponding to a yield of 97.8% of theory; b.p. 85° C./4 Pa; nD20 =1.5666.

後処理

  1. additionAfter completion of the dropwise addition
  2. customis separated in a separating funnel
  3. customThe toluene with the unreacted isobutyraldehyde and residual water is then removed by rotation in a water-jet vacuum
  4. distillationthe residue is distilled in an oil-pump vacuum

出典と根拠

ORDレコード
ord-f58c8ad04f564144b885d3481a4c64b3
出典データセット
uspto-grants-1980_11
特許番号
US04231962

反応ノート

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