Triethylamine → HCID 178428636, 화합물

HRID 274959노트

반응식

HRID 274959 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 178428636HCID 178428636, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-380a404e2f034ca6b2b6f1c617f70f41
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05391556

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