Carbamic acid, ethyl ester → (9H-Xanthene-9-carbonyl)-carbamic acid ethyl ester

HRID 991193ノート

反応式

HRID 991193 の反応式
[NH2:1][C:2]([O:4][CH2:5][CH3:6])=[O:3].[CH:7]1[C:20]2[CH:19]([C:21](Cl)=[O:22])[C:18]3[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=3)[O:12][C:11]=2[CH:10]=[CH:9][CH:8]=1>CN(C1C=CN=CC=1)C.N1C=CC=CC=1>[CH2:5]([O:4][C:2](=[O:3])[NH:1][C:21]([CH:19]1[C:20]2[CH:7]=[CH:8][CH:9]=[CH:10][C:11]=2[O:12][C:13]2[C:18]1=[CH:17][CH:16]=[CH:15][CH:14]=2)=[O:22])[CH3:6]

参加物

5

反応物 2

HCID 5641Carbamic acid, ethyl esterHCID 27608929H-xanthene-9-carbonyl chloride

生成物 1

HCID 9839180(9H-Xanthene-9-carbonyl)-carbamic acid ethyl ester収率 67%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 1049Pyridine溶媒

実験手順

To a stirred solution of urethane (0.82 g, 9.21 mmol) and DMAP (0.05 g, 0.41 mmol) in pyridine (10 ml) was added at 0° C. 9H-xanthene-9-carbonyl chloride (1.50 g, 6.13 mmol). Stirring was continued at RT for 17 h, the reaction mixture was evaporated and water (50 ml)/sat. NaHCO3 solution (20 ml) was added. The solid was filtered off and crystallized from water and afterwards from EtOH/hexane to give the product (1.22 g, 67%) as a white solid, m.p. 228° C. (dec.) and MS: m/e=298.2 (M+H+).

後処理

  1. customthe reaction mixture was evaporated
  2. additionNaHCO3 solution (20 ml) was added
  3. filtrationThe solid was filtered off
  4. customcrystallized from water and afterwards from EtOH/hexane

出典と根拠

ORDレコード
ord-a3a3fc570bf74b60a1070fa7b428c1f0
出典データセット
uspto-grants-2002_10
特許番号
US06462198B1

反応ノート

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