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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Triethylamine → 4-(((6S,9aS)-1-(Benzylcarbamoyl)-8-((6-(3-(4-ethylpiperazin-1-yl)azetidin-1-yl)pyridin-2-yl)methyl)-4,7-dioxo-2-(prop-2-en-1-yl)-octahydro-1H-pyrazino[2,1-c][1,2,4]triazin-6-yl)methyl)-3-fluorophenyl dihydrogen phosphate

HRID 707529
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HRID 707529 반응식
[P:1](Cl)(Cl)(Cl)=[O:2].[CH2:6]([NH:13][C:14]([N:16]1[C@H:21]2[CH2:22][N:23]([CH2:36][C:37]3[CH:42]=[CH:41][CH:40]=[C:39]([N:43]4[CH2:46][CH:45]([N:47]5[CH2:52][CH2:51][N:50]([CH2:53][CH3:54])[CH2:49][CH2:48]5)[CH2:44]4)[N:38]=3)[C:24](=[O:35])[C@H:25]([CH2:26][C:27]3[CH:32]=[CH:31][C:30]([OH:33])=[CH:29][C:28]=3[F:34])[N:20]2[C:19](=[O:55])[CH2:18][N:17]1[CH2:56][CH:57]=[CH2:58])=[O:15])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.C(N(CC)CC)C.[OH-:66].[Na+].C(OCC)(=[O:70])C>O.C1COCC1>[P:1]([OH:2])([OH:70])([O:33][C:30]1[CH:31]=[CH:32][C:27]([CH2:26][C@@H:25]2[N:20]3[C@@H:21]([N:16]([C:14](=[O:15])[NH:13][CH2:6][C:7]4[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=4)[N:17]([CH2:56][CH:57]=[CH2:58])[CH2:18][C:19]3=[O:55])[CH2:22][N:23]([CH2:36][C:37]3[CH:42]=[CH:41][CH:40]=[C:39]([N:43]4[CH2:46][CH:45]([N:47]5[CH2:52][CH2:51][N:50]([CH2:53][CH3:54])[CH2:49][CH2:48]5)[CH2:44]4)[N:38]=3)[C:24]2=[O:35])=[C:28]([F:34])[CH:29]=1)=[O:66]
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참가 물질

8

반응물 5

HCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 14798Sodium HydroxideHCID 24813Phosphorus oxychlorideHCID 91810345E-7386

생성물 1

HCID 118162442
4-(((6S,9aS)-1-(Benzylcarbamoyl)-8-((6-(3-(4-ethylpiperazin-1-yl)azetidin-1-yl)pyridin-2-yl)methyl)-4,7-dioxo-2-(prop-2-en-1-yl)-octahydro-1H-pyrazino[2,1-c][1,2,4]triazin-6-yl)methyl)-3-fluorophenyl dihydrogen phosphate
수율 79%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매2회

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온도
-15 °C

실험 절차

To a mixed solution of phosphorus oxychloride (257 μL, 2.76 mmol) and THF (10.0 mL) was dropwisely added a mixed solution of (6S,9aS)-N-benzyl-8-((6-(3-(4-ethylpiperazin-1-yl)azetidin-1-yl)pyridin-2-yl)methyl)-6-((2-fluoro-4-hydroxyphenyl)methyl)-4,7-dioxo-2-(prop-2-en-1-yl)-octahydro-1H-pyrazino[2,1-c][1,2,4]triazine-1-carboxamide (1.00 g, 1.38 mmol) described in Example 1, triethylamine (768 μL, 5.52 mmol) and THF (10.0 mL) over 10 minutes under a nitrogen atmosphere at −15° C. or lower. The reaction mixture was stirred at −15° C. or lower for 1 hour and 10 minutes. To the reaction mixture was dropwisely added a mixed solution of a 5 N aqueous sodium hydroxide solution (2.03 mL, 10.1 mmol) and water (21.0 mL) over 5 minutes at 10° C. or lower. The reaction mixture was stirred at room temperature for 35 minutes, then ethyl acetate was added to the reaction mixture, and then the resultant solution was partitioned. An aqueous layer was further washed with ethyl acetate, and then 5 N hydrochloric acid was added to the solution to adjust the pH value of the solution at a neutral value. The solvent was distilled away from the reaction mixture under a reduced pressure. Dichloromethane, ethanol and methanol were added to the resultant residue and then stirred, and then the resultant suspension was filtrated using Celite. The solvent was distilled away from the filtrate under a reduced pressure, and the resultant residue was purified by ODS silica gel column chromatography (elution solvent: water/methanol) to give the title compound (881 mg, yield: 79%).

후처리

  1. stirringThe reaction mixture was stirred at room temperature for 35 minutes
  2. customthe resultant solution was partitioned
  3. washAn aqueous layer was further washed with ethyl acetate
  4. addition5 N hydrochloric acid was added to the solution
  5. distillationThe solvent was distilled away from the reaction mixture under a reduced pressure
  6. additionDichloromethane, ethanol and methanol were added to the resultant residue
  7. stirringstirred
  8. filtrationthe resultant suspension was filtrated
  9. distillationThe solvent was distilled away from the filtrate under a reduced pressure
  10. customthe resultant residue was purified by ODS silica gel column chromatography (elution solvent: water/methanol)

출처 및 근거

ORD 기록
ord-0c4efebff6dd4b1ea527a11b0812fb7d
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09174998B2

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