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Chloroform → HCID 59398179, 화합물

HRID 39943
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HRID 39943 반응식
C(Cl)(Cl)Cl.[O:5]1[C:10]2[CH:11]=[CH:12][C:13]([CH2:15][N:16]([CH:24]3[CH2:29][CH2:28][N:27]([CH2:30][CH2:31][N:32]4[C:41]5[C:36](=[C:37]([NH2:42])[CH:38]=[CH:39][CH:40]=5)[CH:35]=[CH:34][C:33]4=[O:43])[CH2:26][CH2:25]3)[C:17](=[O:23])[O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[CH:14][C:9]=2[O:8][CH2:7][CH2:6]1.Cl[C:45]([O:47][CH3:48])=[O:46]>C(N(CC)CC)C>[CH3:48][O:47][C:45](=[O:46])[NH:42][C:37]1[CH:38]=[CH:39][CH:40]=[C:41]2[C:36]=1[CH:35]=[CH:34][C:33](=[O:43])[N:32]2[CH2:31][CH2:30][N:27]1[CH2:28][CH2:29][CH:24]([N:16]([C:17]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:23])[CH2:15][C:13]2[CH:12]=[CH:11][C:10]3[O:5][CH2:6][CH2:7][O:8][C:9]=3[CH:14]=2)[CH2:25][CH2:26]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6212ChloroformHCID 6586Methyl chloroformate2회HCID 59397938HCID 59397938, 화합물

생성물 1

HCID 59398179HCID 59398179, 화합물수율 45.1%

시약·촉매·용매 1

HCID 8471Triethylamine용매2회

실험 절차

To 2 mL of a chloroform solution containing 80 mg of tert-butyl (2,3-dihydro-1,4-benzodioxin-6-ylmethyl)(1-(2-(5-amino-2-oxoquinolin-1(2H)-yl)ethyl)piperidin-4-yl)carbamate, 45 mg of triethylamine and 42 mg of methyl chloroformate were added, and stirred at room temperature for 3 days. To the reaction mixture, 225 mg of triethylamine and 210 mg of methyl chloroformate were added, and stirred at room temperature overnight. The reaction mixture was purified by silica gel column chromatography [Silica Gel; Fuji Silysia Chemical Ltd., Chromatorex-NH, eluent; hexane:ethyl acetate=1:4], to give 40 mg of N-(1-(2-(4-((tert-butoxycarbonyl) (2,3-dihydro-1,4-benzodioxin-6-ylmethyl)amino)piperidin-1-yl)ethyl)-2-oxo-1,2-dihydroquinolin-5-yl)carbamic acid methyl ester as a pale yellow oil.

후처리

  1. additionwere added
  2. stirringstirred at room temperature overnight
  3. customThe reaction mixture was purified by silica gel column chromatography [Silica Gel; Fuji Silysia Chemical Ltd., Chromatorex-NH, eluent; hexane:ethyl acetate=1:4]

출처 및 근거

ORD 기록
ord-9e7c13ec699a496bb0597c4a079f0230
출처 데이터셋
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08524738B2

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