Triethylamine → HCID 178428636、化合物

HRID 274959ノート

反応式

HRID 274959 の反応式
[NH:1]1[C:5]2[CH:6]=[CH:7][C:8]([CH2:10][CH:11]([NH2:21])[C:12]([N:14]3[CH2:19][CH2:18][CH:17]([CH3:20])[CH2:16][CH2:15]3)=[O:13])=[CH:9][C:4]=2[N:3]=[CH:2]1.C(N(CC)CC)C.[CH3:29][N:30]1[C:42]2[CH2:41][CH2:40][CH2:39][CH2:38][C:37]=2[C:36]2[C:31]1=[CH:32][CH:33]=[C:34]([S:43](Cl)(=[O:45])=[O:44])[CH:35]=2>C(Cl)(Cl)Cl>[NH:1]1[C:5]2[CH:6]=[CH:7][C:8]([CH2:10][CH:11]([NH:21][S:43]([C:34]3[CH:35]=[C:36]4[C:31](=[CH:32][CH:33]=3)[N:30]([CH3:29])[C:42]3[CH2:41][CH2:40][CH2:39][CH2:38][C:37]4=3)(=[O:44])=[O:45])[C:12]([N:14]3[CH2:19][CH2:18][CH:17]([CH3:20])[CH2:16][CH2:15]3)=[O:13])=[CH:9][C:4]=2[N:3]=[CH:2]1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 218061079-Methyl-1,2,3,4-tetrahydro-carbazol-6-sulphonic acid chlorideHCID 178428665HCID 178428665、化合物

生成物 1

HCID 178428636HCID 178428636、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

To a solution of 1 g (0.0034 Mol) of 1-(1H-benzimidazol-5-yl-methyl)-2-(4-methyl-piperidin-1-yl)-2-oxoethylamine and 1.1 g (0.011 Mol) of triethylamine in 30 ml of chloroform are added dropwise, at ambient temperature and with stirring, 0.96 g (0.0034 Mol) of 9-methyl-1,2,3,4-tetrahydro-carbazol-6-sulphonic acid chloride dissolved in 10 ml of chloroform. After 12 hours' stirring the mixture is evaporated down in vacuo and the residue obtained is chromatographed over a silica gel column (eluant: ethyl acetate/methanol=9:1). The eluate having an Rf value of 0.3 is collected and evaporated down in vacuo.

後処理

  1. stirringAfter 12 hours' stirring the mixture
  2. customis evaporated down in vacuo
  3. customthe residue obtained
  4. customis chromatographed over a silica gel column (eluant: ethyl acetate/methanol=9:1)
  5. customis collected
  6. customevaporated down in vacuo

出典と根拠

ORDレコード
ord-380a404e2f034ca6b2b6f1c617f70f41
出典データセット
uspto-grants-1995_02
特許番号
US05391556

反応ノート

読み込み中…