Pyridine → 4-(N,N-diphenylamino)benzyl acetate

HRID 966868

反応式

HRID 966868 の反応式
[C:1]1([N:7]([C:14]2[CH:21]=[CH:20][C:17]([CH2:18][OH:19])=[CH:16][CH:15]=2)[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.N1C=CC=CC=1.[C:28](OC(=O)C)(=[O:30])[CH3:29]>O>[C:28]([O:19][CH2:18][C:17]1[CH:20]=[CH:21][C:14]([N:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[CH:15][CH:16]=1)(=[O:30])[CH3:29]

参加物

5

反応物 3

HCID 1049PyridineHCID 7918Acetic AnhydrideHCID 11323339(4-(Diphenylamino)phenyl)methanol

生成物 1

HCID 222924294-(N,N-diphenylamino)benzyl acetate収率 95%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

4-(N,N-Diphenylamino)benzyl alcohol (5.94 g, 0.0216 mol), pyridine (16 mL) and acetic anhydride (11.4 mL) were mixed in a three-neck flask equipped with a condenser and addition funnel. The resulting mixture was stirred overnight at room temperature. Deionized water (50 mL) was then added and the resulting mixture stirred for 2 hours. The product was obtained by filtration, and recrystallized from hexane to yield the desired product (6.52 g, 95%). m.p. 105-6° C.; 1H NMR δ: 2.10 (s, 3H, CH3), 5.04 (s, 2H, CH2), 7.0-7.4 (m, 14H, phenyl). Analysis: Calculated for C19H17NO2: C, 79.46%; H, 6.03%; N, 4.41%. Found: C, 79.37 %; H, 5.72 %; N, 4.41%.

後処理

  1. customequipped with a condenser and addition funnel
  2. stirringthe resulting mixture stirred for 2 hours
  3. customThe product was obtained by filtration
  4. customrecrystallized from hexane

出典と根拠

ORDレコード
ord-a2298b0577074858bff32220db261a94
出典データセット
uspto-grants-2005_10
特許番号
US06953570B2

関連ノート

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