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Triethylamine → HCID 67204782、化合物

HRID 1626321
ノート
印刷プレビュー

反応式

HRID 1626321 の反応式
Cl[C:2]1[N:10]=[CH:9][N:8]=[C:7]2[C:3]=1[N:4]=[C:5]([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[N:6]2[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.Cl.Cl.[CH3:25][C:26]1[C:31]([CH3:32])=[CH:30][CH:29]=[CH:28][C:27]=1[N:33]1[CH2:38][CH2:37][N:36]([CH2:39][CH2:40][CH2:41][NH2:42])[CH2:35][CH2:34]1.C(N(CC)CC)C>C(O)C>[CH3:25][C:26]1[C:31]([CH3:32])=[CH:30][CH:29]=[CH:28][C:27]=1[N:33]1[CH2:34][CH2:35][N:36]([CH2:39][CH2:40][CH2:41][NH:42][C:2]2[N:10]=[CH:9][N:8]=[C:7]3[C:3]=2[N:4]=[C:5]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[N:6]3[C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH2:37][CH2:38]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

5

反応物 3

HCID 8471TriethylamineHCID 70664367HCID 70664367、化合物HCID 86046565HCID 86046565、化合物

生成物 1

HCID 67204782HCID 67204782、化合物収率 46.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
80 °C

実験手順

To a mixture of 6-chloro-8,9-diphenyl-9H-purine (150 mg, 0.49 mmol) and 3-(4-(2,3-dimethylphenyl)piperazin-1-yl)propan-1-amine dihydrochloride (313 mg, 0.98 mmol) in ethanol (4.9 mL) was added triethyl amine (0.27 mL, 1.96 mmol) and stirred at 80° C. for 15 hrs. The resulting reaction mixture was concentrated under reduced pressure. The residue was diluted with CH2Cl2, and washed with water. The organic layer thus separated was dried over anhydrous MgSO4, filtered, and concentrated in vacuo. The crude product thus obtained was purified by preparative HPLC (purification system, Gilson) to provide the title compound (117 mg) as a white solid.

後処理

  1. customThe resulting reaction mixture
  2. concentrationwas concentrated under reduced pressure
  3. additionThe residue was diluted with CH2Cl2
  4. washwashed with water
  5. customThe organic layer thus separated
  6. dry with materialwas dried over anhydrous MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customThe crude product thus obtained
  10. customwas purified by preparative HPLC (purification system, Gilson)

出典と根拠

ORDレコード
ord-a7a025d91abc4fa69d2e2c0937649b25
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08785453B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート