Triethylamine → N-[4-[3-(1-piperidinylmethyl)phenoxy]-2-butenyl]-1,3,4-thiadiazole-2,5-diamine

HRID 4636

反応式

HRID 4636 の反応式
[N:1]1([CH2:7][C:8]2[CH:9]=[C:10]([CH:17]=[CH:18][CH:19]=2)[O:11][CH2:12][CH:13]=[CH:14][CH2:15][NH2:16])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C(N(CC)CC)C.Br[C:28]1[S:32][C:31]([NH2:33])=[N:30][N:29]=1>C1COCC1>[N:1]1([CH2:7][C:8]2[CH:9]=[C:10]([CH:17]=[CH:18][CH:19]=2)[O:11][CH2:12][CH:13]=[CH:14][CH2:15][NH:16][C:28]2[S:32][C:31]([NH2:33])=[N:30][N:29]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 36508832-Amino-5-bromo-1,3,4-thiadiazoleHCID 544322804-[3-(1-Piperidinylmethyl)phenoxy]2-butene-1-amine

生成物 1

HCID 54123024N-[4-[3-(1-piperidinylmethyl)phenoxy]-2-butenyl]-1,3,4-thiadiazole-2,5-diamine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

0.6 g (2.3 mmol) of 4-[3-(1-piperidinylmethyl)phenoxy]2-butene-1-amine, 0.35 ml of triethylamine and 0.42 g (2.3 mmol) of 5-bromo-1,3,4-thiadiazole-2-amin are heated under reflux in 20 ml of THF for 3 hours. Solid triethylammonium bromide is filtered off, the filtrate is concentrated by evaporation and the oily residue is purified by preparative layer chromatography.

後処理

  1. filtrationSolid triethylammonium bromide is filtered off
  2. concentrationthe filtrate is concentrated by evaporation
  3. customthe oily residue is purified by preparative layer chromatography

出典と根拠

ORDレコード
ord-8eb4fc42e2804d748fd87ba8aac6a162
出典データセット
uspto-grants-1988_02
特許番号
US04727081

関連ノート

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