2-(Methylamino)ethanol → HCID 58024773, 화합물

HRID 1675677노트

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HRID 1675677 반응식
Br[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][C:9]([NH:11][C:12]1[CH:20]=[CH:19][C:15]([C:16]([OH:18])=[O:17])=[CH:14][CH:13]=1)=[O:10].[CH3:21][NH:22][CH2:23][CH2:24][OH:25].C(N(CC)C(C)C)(C)C>CN(C)C=O>[OH:25][CH2:24][CH2:23][N:22]([CH3:21])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][C:9]([NH:11][C:12]1[CH:20]=[CH:19][C:15]([C:16]([OH:18])=[O:17])=[CH:14][CH:13]=1)=[O:10]

참가 물질

5

반응물 3

HCID 80162-(Methylamino)ethanolHCID 81531DiisopropylethylamineHCID 58024763HCID 58024763, 화합물2회

생성물 1

HCID 58024773HCID 58024773, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
60 °C

실험 절차

To a mixture of 4-[(8-bromooctanoyl)amino]benzoic acid (50 mg, 0.15 mmol, as prepared in Intermediate 36) in N,N-dimethylformamide (2 ml) was added 2-(methylamino)ethanol (24 microliters, 0.3 mmol, 2 equivalents, commercially available e.g. from Aldrich) followed by N,N-diisopropylethylamine (0.13 mL, 0.8 mmol, about 5 equivalents), and the resulting solution was heated at 60° C. for 16 hours. The solvent was removed by evaporation, and the residue was purified by Mass Directed Automated Preparative HPLC (Method A). Fractions containing product were pooled and evaporated to dryness to give the title compound (25.4 mg) as a pale brown solid. LCMS showed MH+=337; TRET=2.03 min.

후처리

  1. customThe solvent was removed by evaporation
  2. customthe residue was purified by Mass Directed Automated Preparative HPLC (Method A)
  3. additionFractions containing product
  4. customevaporated to dryness

출처 및 근거

ORD 기록
ord-9055e0d2dd4b4569bbd77ee3a8d6071e
출처 데이터셋
uspto-grants-2011_08
특허 번호
US08003663B2

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