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Triethylamine → 2-[4-(2-(1,3-Dioxolan-2-yl)-ethyl)-1-piperazinyl]-1-phenyl indole 3-carboxylic acid (4-methyl)-piperazide

HRID 26208
ノート
印刷プレビュー

反応式

HRID 26208 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8]([C:10]2[C:18]3[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=3)[N:12]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[C:11]=2[N:25]2[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]2)=[O:9])[CH2:4][CH2:3]1.Cl[CH2:32][CH2:33][CH:34]1[O:38][CH2:37][CH2:36][O:35]1.C(N(CC)CC)C.C1(N)C(F)=C(F)C(F)=C(N)C=1F.Cl.Cl>C1(C)C=CC=CC=1.C(Cl)(Cl)Cl>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([C:8]([C:10]2[C:18]3[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=3)[N:12]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[C:11]=2[N:25]2[CH2:26][CH2:27][N:28]([CH2:32][CH2:33][CH:34]3[O:38][CH2:37][CH2:36][O:35]3)[CH2:29][CH2:30]2)=[O:9])[CH2:6][CH2:7]1
参加物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 8471TriethylamineHCID 780712-(2-Chloroethyl)-1,3-dioxolaneHCID 149026Tetrafluoro-m-phenylenediamine dihydrochlorideHCID 867364551-Phenyl-2-(1-piperazinyl)-indole 3-carboxylic acid (4-methyl)-Piperazide

生成物 1

HCID 867364582-[4-(2-(1,3-Dioxolan-2-yl)-ethyl)-1-piperazinyl]-1-phenyl indole 3-carboxylic acid (4-methyl)-piperazide

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 6212Chloroform溶媒

実験手順

A stirred mixture of 8 g (0.02 mol) of 1-phenyl-2-(1-piperazinyl)-indole 3-carboxylic acid (4-methyl)-piperazide, 9.45 g (0.07 mol) of 2-(2-chloroethyl)-1,3-dioxolane and 9.7 ml of triethylamine in 60 ml of toluene was maintained at the boil for 40 hours. After cooling, the mixture was diluted with 200 ml of chloroform, washed three times with water, and the solvent was eliminated in vacuo. The resinous residue of the organic phase was chromatographed using silica gel 60 (0.06-0.2 mm, deactivated by 10% of water, column size: 3 × 100 cm) with chloroform containing 10% methanol. The base was eluted as a resin. The yield amounted to 6.6 g (66% of the theoretical yield). The dihydrochloride melted at 215°-217° C.

後処理

  1. temperaturewas maintained at the boil for 40 hours
  2. temperatureAfter cooling
  3. washwashed three times with water
  4. customThe resinous residue of the organic phase was chromatographed
  5. washThe base was eluted as a resin
  6. customtheoretical yield)

出典と根拠

ORDレコード
ord-2ea726274d5b438283d3b7d1fe3bc327
出典データセット
uspto-grants-1979_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04148895

反応ノート

読み込み中…

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