Water → N-isobutylidene-3-phenoxybenzylamine

HRID 224268노트

반응식

HRID 224268 반응식
[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]

참가 물질

5

반응물 3

HCID 962WaterHCID 6561IsobutyraldehydeHCID 10948363-Phenoxy-benzylamine

생성물 1

HCID 23332476N-isobutylidene-3-phenoxybenzylamine수율 98%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f58c8ad04f564144b885d3481a4c64b3
출처 데이터셋
uspto-grants-1980_11
특허 번호
US04231962

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