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Triethylamine → HCID 22711097, 화합물

HRID 352972
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HRID 352972 반응식
FC(F)(F)C(O)=O.[Cl:8][C:9]1[CH:10]=[C:11]2[C:15](=[CH:16][CH:17]=1)[NH:14][C:13]([S:18]([N:21]1[CH2:26][CH2:25][N:24]([C:27]([C:29]3[S:30][C:31]4[CH2:32][NH:33][CH2:34][CH2:35][C:36]=4[N:37]=3)=[O:28])[CH:23]([CH2:38][C:39]([NH:41][S:42]([CH3:45])(=[O:44])=[O:43])=[O:40])[CH2:22]1)(=[O:20])=[O:19])=[CH:12]2.C(N(CC)CC)C.[C:53](=O)([O:61]C1C=CC([N+]([O-])=O)=CC=1)[O:54][CH:55]([O:57][C:58](=[O:60])[CH3:59])[CH3:56]>C(O)C>[C:58]([O:57][CH:55]([O:54][C:53]([CH:34]1[NH:33][CH2:32][C:31]2[S:30][C:29]([C:27]([N:24]3[CH2:25][CH2:26][N:21]([S:18]([C:13]4[NH:14][C:15]5[C:11]([CH:12]=4)=[CH:10][C:9]([Cl:8])=[CH:17][CH:16]=5)(=[O:20])=[O:19])[CH2:22][CH:23]3[CH2:38][C:39]([NH:41][S:42]([CH3:45])(=[O:44])=[O:43])=[O:40])=[O:28])=[N:37][C:36]=2[CH2:35]1)=[O:61])[CH3:56])(=[O:60])[CH3:59]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 117805601-acetoxyethyl p-nitrophenyl carbonateHCID 22711201HCID 22711201, 화합물

생성물 1

HCID 22711097HCID 22711097, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

In ethanol (2 ml) was dissolved N-[[4-[(5-chloroindol-2-yl)sulfonyl]-1-[(4,5,6,7-tetrahydrothiazolo[5,4-c]pyridin-2-yl)carbonyl]piperazin-2-yl]acetyl]methanesulfonamide trifluoroacetate (97 mg), followed by the addition of triethylamine (0.63 ml) and 1-acetoxyethyl p-nitrophenyl carbonate (110 mg). The resulting mixture was stirred at room temperature for 4 hours. The reaction mixture was concentrated under reduced pressure. Methylene chloride was added to the residue. The resulting mixture was washed with water, dried over anhydrous sodium sulfate and distilled to remove the solvent. The residue was purified by chromatography on a silica gel column (methylene chloride:methanol=50:1), whereby the title compound (50 mg) was obtained as a colorless foam.

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. additionMethylene chloride was added to the residue
  3. washThe resulting mixture was washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationdistilled
  6. customto remove the solvent
  7. customThe residue was purified by chromatography on a silica gel column (methylene chloride:methanol=50:1), whereby the title compound (50 mg)
  8. customwas obtained as a colorless foam

출처 및 근거

ORD 기록
ord-9f25f77afe4e4b8393e4d04dfcfee96e
출처 데이터셋
uspto-grants-2004_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06747023B1

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