Triethylamine → HCID 86681323, 화합물

HRID 1430296

반응식

HRID 1430296 반응식
Cl.[NH2:2][C:3]1([C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1.C(N(CC)CC)C.Br[CH2:22][CH2:23][O:24][CH2:25][CH2:26]Br>CN(C)C=O.C(OCC)(=O)C>[O:24]1[CH2:25][CH2:26][N:2]([C:3]2([C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]2)[CH2:22][CH2:23]1

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 21521Bis(2-bromoethyl) etherHCID 11241228Ethyl 1-aminocyclohexane-1-carboxylate hydrochloride

생성물 1

HCID 86681323HCID 86681323, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

Ethyl 1-aminocyclohexancarboxylate hydrogen chloride (5.800 g), triethylamine (13.62 mL) and 1-bromo-2-(2-bromoethoxy)ethane (4.21 mL) were stirred together in N,N-dimethylformamide (50 mL) at 95° C. overnight. The reaction mixture was diluted with ethyl acetate (150 mL), washed with water (100 mL) and brine (100 mL), dried over magnesium sulfate, filtered, and concentrated. Silica gel chromatography eluting with a gradient of 5% to 25% ethyl acetate/hexanes provided the title compound.

후처리

  1. washwashed with water (100 mL) and brine (100 mL)
  2. dry with materialdried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. washSilica gel chromatography eluting with a gradient of 5% to 25% ethyl acetate/hexanes

출처 및 근거

ORD 기록
ord-fb5412b24ac84b32bf114eacb4a68bbe
출처 데이터셋
uspto-grants-2015_01
특허 번호
US08940737B2

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