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Water → HCID 11719782、化合物

HRID 1695520
ノート
印刷プレビュー

反応式

HRID 1695520 の反応式
[O:1]([C:8]1[CH:14]=[CH:13][C:11]([NH2:12])=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:15](N1C=CN=C1)(N1C=CN=C1)=[O:16].[C@H:27]1([CH2:37][O:38][C:39]2[CH:44]=[CH:43][C:42]([NH2:45])=[CH:41][CH:40]=2)[C@@H:36]2[N:31]([CH2:32][CH2:33][CH2:34][CH2:35]2)[CH2:30][CH2:29][CH2:28]1.O>CN(C=O)C>[C@H:27]1([CH2:37][O:38][C:39]2[CH:44]=[CH:43][C:42]([NH:45][C:15]([NH:12][C:11]3[CH:10]=[CH:9][C:8]([O:1][C:2]4[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=4)=[CH:14][CH:13]=3)=[O:16])=[CH:41][CH:40]=2)[C@@H:36]2[N:31]([CH2:32][CH2:33][CH2:34][CH2:35]2)[CH2:30][CH2:29][CH2:28]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 8764(4-Aminophenoxy)benzeneHCID 682631,1'-CarbonyldiimidazoleHCID 66879100HCID 66879100、化合物

生成物 1

HCID 11719782HCID 11719782、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒3 回

実験手順

A solution of 4-phenoxyaniline (185 mg) in DMF (1 ml) was added dropwise to a solution, cooled to 0° C., of carbonyldiimidazole (162 mg) in DMF (1 ml). After 30 minutes, 4-[(1R,9aR)-1-(octahydroquinolizin-1-yl)-methoxy]-phenylamine (289 mg) in DMF (1 ml) was added dropwise. The reaction solution was kept firstly at room temperature for 2 hours and then at 80° C. for 30 minutes. The mixture was added dropwise to water (20 ml), and the resulting precipitate was filtered off with suction and washed with water. Alternatively, the product can also be extracted with ethyl acetate and purified after concentration by chromatography. The product with the molecular weight of 471.60 (C29H33N3O3); MS (ESI): 472 (M+H+) was obtained in this way.

後処理

  1. waitThe reaction solution was kept firstly at room temperature for 2 hours
  2. waitat 80° C. for 30 minutes
  3. filtrationthe resulting precipitate was filtered off with suction
  4. washwashed with water
  5. extractionAlternatively, the product can also be extracted with ethyl acetate
  6. custompurified
  7. concentrationafter concentration by chromatography
  8. customMS (ESI): 472 (M+H+) was obtained in this way

出典と根拠

ORDレコード
ord-5026103ee0cd4b1984ecbd3fece85763
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08163741B2

反応ノート

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