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Benzoyl chloride → HCID 18596283、化合物

HRID 1247914
ノート
印刷プレビュー

反応式

HRID 1247914 の反応式
[NH2:1][C:2]1[N:3]=[CH:4][C:5]2[CH2:14][C@H:13]3[C@@H:8]([CH2:9][CH2:10][CH2:11][N:12]3[CH2:15][CH2:16][CH3:17])[CH2:7][C:6]=2[N:18]=1.[C:19]([Cl:27])(=[O:26])[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>N1C=CC=CC=1>[ClH:27].[ClH:27].[C:19]([NH:1][C:2]1[N:3]=[CH:4][C:5]2[CH2:14][C@H:13]3[C@@H:8]([CH2:9][CH2:10][CH2:11][N:12]3[CH2:15][CH2:16][CH3:17])[CH2:7][C:6]=2[N:18]=1)(=[O:26])[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 7412Benzoyl chlorideHCID 18596256HCID 18596256、化合物

生成物 1

HCID 18596283HCID 18596283、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

Following the above procedure, trans-(±)-2-amino-6-n-propyl-5,5a,6,7,8,9,9a,10-octahydropyrimido[4,5-g]quinoline was reacted with benzoyl chloride in pyridine solution. The residue obtained after working up the reaction mixture as indicated above was chromatographed over florisil using chloroform with increasing amounts (0-10%) of methanol as the eluant. Fraction ten contained the desired 2-benzoylamino compound (by TLC). The solvent was removed therefrom in vacuo. The resulting residue was dissolved in ethanol and gaseous hydrogen chloride passed into the ethanol solution. Addition of ether to the point of incipient precipitation yielded trans-(±)-2-benzoylamino-6-n-propyl-5,5a,6,7,8,9,9a,10-octahydropyrimido[4,5-g]quinoline dihydrochloride; molecular ion at 350.

後処理

  1. customThe residue obtained
  2. customabove was chromatographed over florisil
  3. customThe solvent was removed
  4. dissolutionThe resulting residue was dissolved in ethanol
  5. additionAddition of ether
  6. customto the point of incipient precipitation

出典と根拠

ORDレコード
ord-44f87cdabc32487091eb20c17cbf0979
出典データセット
uspto-grants-1985_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04521421

反応ノート

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