Sodium Iodide → HCID 68538779、化合物

HRID 2389318ノート

反応式

HRID 2389318 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([O:8][CH2:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[C:3]=1[NH:16][C:17](=[O:19])[CH3:18].Br[CH2:21][C:22]([O:24][CH2:25][CH3:26])=[O:23].[I-].[Na+].C([O-])([O-])=O.[K+].[K+]>CN(C=O)C.O>[C:17]([NH:16][C:3]1[C:4]([O:8][CH2:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[CH:5][CH:6]=[CH:7][C:2]=1[NH:1][CH2:21][C:22]([O:24][CH2:25][CH3:26])=[O:23])(=[O:19])[CH3:18]

参加物

7

反応物 4

HCID 5238Sodium IodideHCID 7748Ethyl bromoacetateHCID 11430Potassium CarbonateHCID 68538324HCID 68538324、化合物

生成物 1

HCID 68538779HCID 68538779、化合物収率 72.6%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

To a mixture of N-[2-amino-6-(benzyloxy)phenyl]acetamide (2.95 g) and ethyl bromoacetate (2.11 g) in DMF (29.5 mL) were added sodium iodide (1.73 g) and K2CO3 (1.91 g) at ambient temperature. The mixture was stirred at 80° C. for 6 hours. After cooling, the reaction mixture was added water (50 mL). The formed precipitate was collected by filteration and washed with water and recrystallized from solvent (EtOAc and n-hexane) to give ethyl N-[2-acetamido-3-(benzyloxy)phenyl]glycinate (2.86 g) as a white solid.

後処理

  1. temperatureAfter cooling
  2. customThe formed precipitate was collected by filteration
  3. washwashed with water
  4. customrecrystallized from solvent (EtOAc and n-hexane)

出典と根拠

ORDレコード
ord-f2ea4840a7ff4ef4966d51d9f4f7d93d
出典データセット
uspto-grants-2012_09
特許番号
US08273745B2

反応ノート

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