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Trifluoroacetic acid → HCID 21873402、化合物

HRID 723354
ノート
印刷プレビュー

反応式

HRID 723354 の反応式
[C:1](N1C=CN=C1)(N1C=CN=C1)=[O:2].[C:13]1([CH3:27])[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=1[O:19][C:20]1[CH:25]=[CH:24][C:23]([NH2:26])=[CH:22][CH:21]=1.CO[CH:30](OC)[CH2:31][NH:32][C:33]1[CH:38]=[CH:37][C:36]([O:39][CH2:40][CH2:41][N:42]([CH3:44])[CH3:43])=[CH:35][CH:34]=1.FC(F)(F)C(O)=O>CN(C)C=O.C(OCC)(=O)C>[CH3:44][N:42]([CH3:43])[CH2:41][CH2:40][O:39][C:36]1[CH:35]=[CH:34][C:33]([N:32]2[CH:31]=[CH:30][N:26]([C:23]3[CH:22]=[CH:21][C:20]([O:19][C:14]4[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=4[CH3:27])=[CH:25][CH:24]=3)[C:1]2=[O:2])=[CH:38][CH:37]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 6422Trifluoroacetic acidHCID 682631,1'-CarbonyldiimidazoleHCID 925054-(o-Tolyloxy)anilineHCID 21873475HCID 21873475、化合物

生成物 1

HCID 21873402HCID 21873402、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒
HCID 8857
Ethyl Acetate
溶媒

反応条件

温度
80 °C

実験手順

Carbonyldiimidazole (40 mg) was added to a solution of 4-o-tolyloxyphenylamine (50 mg) in dimethylformamide (2 mL) at 0° C. After 30 minutes, (2,2-dimethoxyethyl)-[4-(2-dimethylaminoethoxy)phenyl]amine (67 mg) was added, and the mixture was heated at 80° C. for 2 hours. After cooling to room temperature, trifluoroacetic acid (0.5 mL) was added and the mixture was left to stand for 72 hours. The reaction solution was diluted with ethyl acetate and washed with saturated sodium bicarbonate solution. The organic phase was dried and concentrated. The residue was purified by preparative HPLC. The product with the molecular weight of 429.52 (C26H27N3O3); MS (ESI): 430 ([M+H]+), was obtained as hydrotrifluoroacetate in this way.

後処理

  1. temperatureAfter cooling to room temperature
  2. waitthe mixture was left
  3. waitto stand for 72 hours
  4. washwashed with saturated sodium bicarbonate solution
  5. customThe organic phase was dried
  6. concentrationconcentrated
  7. customThe residue was purified by preparative HPLC
  8. customMS (ESI): 430 ([M+H]+), was obtained as hydrotrifluoroacetate in this way

出典と根拠

ORDレコード
ord-a46f2375f0a44419bf14d3bde4c87df0
出典データセット
uspto-grants-2006_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07141561B2

反応ノート

読み込み中…

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