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Triethylamine → Triethylamine hydrochloride

HRID 1978408
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HRID 1978408 반응식
CS(O[CH2:6][C@H:7]1[O:12][C:11]2[CH:13]=[CH:14][CH:15]=[CH:16][C:10]=2[O:9][CH2:8]1)(=O)=O.[ClH:17].Cl.[NH:19]1[CH2:24][CH2:23][CH:22]([CH2:25][NH:26][C:27]([C:29]2[S:39][C:38]3[N:40]4[C:31](=[CH:32][N:33]=[C:34]4[CH:35]=[CH:36][CH:37]=3)[CH:30]=2)=[O:28])[CH2:21][CH2:20]1.[CH2:41]([N:43]([CH2:46][CH3:47])[CH2:44][CH3:45])[CH3:42]>C(O)C>[O:12]1[C:11]2[CH:13]=[CH:14][CH:15]=[CH:16][C:10]=2[O:9][CH2:8][C@H:7]1[CH2:6][N:19]1[CH2:24][CH2:23][CH:22]([CH2:25][NH:26][C:27]([C:29]2[S:39][C:38]3[N:40]4[C:31](=[CH:32][N:33]=[C:34]4[CH:35]=[CH:36][CH:37]=3)[CH:30]=2)=[O:28])[CH2:21][CH2:20]1.[ClH:17].[CH2:41]([N:43]([CH2:46][CH3:47])[CH2:44][CH3:45])[CH3:42]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 11128529(S)-(2,3-Dihydrobenzo[b][1,4]dioxin-2-yl)methyl methanesulfonateHCID 21993937N-(piperidin-4-ylmethyl)-5-thia-1,8b-diazaacenaphthylene-4-carboxamide dihydrochloride

생성물 2

HCID 11130Triethylamine hydrochlorideHCID 9804407(R)-N-[1-(1,4-benzodioxan-2-ylmethyl)piperidin-4-ylmethyl)-5-thia-1,8b-diazaacenaphthylene-4-carboxamide

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of the above crude (S)-2-methanesulfonyloxymethyl-1,4-benzodioxane, 1.05 g (2.71 mM) of N-(piperidin-4-ylmethyl)-5-thia-1,8b-diazaacenaphthylene-4-carboxamide dihydrochloride, and 1.20 ml (8.64 mM) of triethylamine in 30 ml of ethanol was refluxed for 3 days. The solvent was then distilled off under reduced pressure and the residue was purified by silica gel column chromatography (ethyl acetate to ethyl acetate-methanol=4/1 to 3/1) to provide the title compound and triethylamine hydrochloride as a mixture. This mixture was diluted with ethyl acetate and washed serially with aqueous solution of sodium hydrogen carbonate, water, and saturated aqueous solution of NaCl. The organic layer was dried over MgSO4 and the solvent was distilled off to provide the title compound.

후처리

  1. distillationThe solvent was then distilled off under reduced pressure
  2. customthe residue was purified by silica gel column chromatography (ethyl acetate to ethyl acetate-methanol=4/1 to 3/1)

출처 및 근거

ORD 기록
ord-c467df2bb67546778ec33b7939480055
출처 데이터셋
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06235731B1

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