Triethylamine → HCID 69455767, 화합물

HRID 2370920노트

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HRID 2370920 반응식
[NH2:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][CH:9]([C:15]2[N:16]=[CH:17][NH:18][CH:19]=2)[C:10]([O:12][CH2:13][CH3:14])=[O:11])=[CH:4][CH:3]=1.Br[CH:21]1[CH2:26][CH2:25][N:24]([C:27]([O:29][CH2:30][C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)=[O:28])[CH2:23][CH2:22]1.C(N(CC)CC)C.CC(=O)OCC.O>C1COCC1>[NH2:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][CH:9]([C:15]2[N:16]=[CH:17][N:18]([CH:21]3[CH2:26][CH2:25][N:24]([C:27]([O:29][CH2:30][C:31]4[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=4)=[O:28])[CH2:23][CH2:22]3)[CH:19]=2)[C:10]([O:12][CH2:13][CH3:14])=[O:11])=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 2776275Benzyl 4-bromotetrahydro-1(2H)-pyridinecarboxylateHCID 22728543Water ethylacetateHCID 178470993HCID 178470993, 화합물

생성물 1

HCID 69455767HCID 69455767, 화합물수율 30%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 60.1 mg (0.23 mmol) of the compound from example 1g, 68.9 mg (0.23 mol) of 4-bromo-1-benzyloxycarbonylpiperidine, 97 μl (0.69 mmol) of triethylamine in 1 ml of absolute THF was treated in a microwave at 180° C. for 2 h. The reaction solution was then mixed with 2 ml of EA/water (1:1), and the EA phase was separated off and dried over Na2SO4. Filtering, stripping off the solvent and purifying the remaining residue by chromatography on RP silica gel with CH3CN/water/0.1% TFA as mobile phase afforded 33 mg of the title compound as bistrifluoroacetate.

후처리

  1. customthe EA phase was separated off
  2. dry with materialdried over Na2SO4
  3. filtrationFiltering
  4. custompurifying the remaining residue by chromatography on RP silica gel with CH3CN/water/0.1% TFA as mobile phase

출처 및 근거

ORD 기록
ord-11efb4951be344c0815461006f9a879d
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08710232B2

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