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Methylamine → HCID 178485529, 화합물

HRID 1014509
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HRID 1014509 반응식
Cl.Cl[C:3]1[N:16]2[C:7](=[N:8][C:9]3[C:14]([C:15]2=[O:17])=[C:13]([F:18])[CH:12]=[CH:11][CH:10]=3)[C:6]2[CH:19]=[CH:20][N:21](S(C3C=CC(C)=CC=3)(=O)=O)[C:5]=2[N:4]=1.[NH2:32][C:33]1[CH:41]=[C:40]2[C:36]([CH2:37][CH2:38][N:39]2[C:42](=[O:47])[C:43]([CH3:46])([OH:45])[CH3:44])=[CH:35][C:34]=1[O:48][CH3:49].[CH3:50][NH2:51].[OH-].[K+]>C1COCC1.C(OCC)(=O)C>[F:18][C:13]1[CH:12]=[CH:11][CH:10]=[C:9]([NH:8][C:7]2[N:16]=[C:3]([NH:32][C:33]3[CH:41]=[C:40]4[C:36]([CH2:37][CH2:38][N:39]4[C:42](=[O:47])[C:43]([OH:45])([CH3:44])[CH3:46])=[CH:35][C:34]=3[O:48][CH3:49])[NH:4][C:5]3=[N:21][CH:20]=[CH:19][C:6]=23)[C:14]=1[C:15]([NH:51][CH3:50])=[O:17]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6329MethylamineHCID 14797Potassium HydroxideHCID 594417381-[6-amino-5-(methyloxy)-2,3-dihydro-1H-indol-1-yl]-2-methyl-1-oxo-2-propanolHCID 673162535-chloro-8-fluoro-3-[(4-methylphenyl)sulfonyl]pyrrolo[2',3':4,5]pyrimido[6,1-b]quinazolin-7(3H)-one HCl salt

생성물 1

HCID 178485529HCID 178485529, 화합물수율 39%

시약·촉매·용매

2
HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

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온도
65 °C

실험 절차

A suspension of 5-chloro-8-fluoro-3-[(4-methylphenyl)sulfonyl]pyrrolo[2′,3′:4,5]pyrimido[6,1-b]quinazolin-7(3H)-one hydrogen chloride (300 mg, 0.63 mmol) and 1-[6-amino-5-(methyloxy)-2,3-dihydro-1H-indol-1-yl]-2-methyl-1-oxo-2-propanol (157 mg, 0.63 mmol) in THF(250 ml) was heated at 65° C. for 4 hrs. The reaction was diluted with ethyl acetate (200 ml) and washed with saturated NaHCO3 (300 ml). Organic layer was removed, concentrated by rotary evaporation, solids triturated from ethyl acetate/hexanes, and dried under house vacuum prior to next step. ESIMS (M+H)+=657. The solids were then added to THF (200 ml) followed by a solution of methylamine (2M in THF, 11.42 ml, 22.84 mmol) and the resulting mixture was stirred at rt overnight. Next, the crude reaction was adsorbed onto silica gel and purified by silica gel chromatography (DCM to 10% MeOH/DCM over 30 min). ESIMS (M+H)+=688. The isolated pure amide was redissolved in 1,4-dioxane (10 ml), and potassium hydroxide (8.72 ml, 8.72 mmol) was added and the reaction was heated in the microwave at 120° C. for 20 min. The resulting solution was adsorbed onto silica gel and purified by silica gel chromatography (DCM to 10% MeOH/DCM) to afford the title compound (0.130 g, 39% over three steps). ESIMS (M+H)+=534. 1H NMR (400 MHz, DMSO-d6) δ ppm 1.38 (s, 6 H) 2.80 (d, J=4.41 Hz, 3 H) 3.06 (t, J=8.03 Hz, 2 H) 3.78 (s, 3 H) 4.43 (t, J=8.23 Hz, 2 H) 5.42 (s, 1 H) 6.26-6.27 (m, 1 H) 6.85-6.93 (m, 1 H) 6.93 (m, 1 H) 6.96 (s, 1 H) 7.28-7.38 (m, 1 H) 7.55 (s, 1 H) 8.37 (d, J=8.43 Hz, 1 H) 8.51-8.58 (m, 1 H) 8.62 (s, 1 H) 10.17 (s, 1 H) 11.26 (s, 1 H).

후처리

  1. washwashed with saturated NaHCO3 (300 ml)
  2. customOrganic layer was removed
  3. concentrationconcentrated by rotary evaporation, solids
  4. customtriturated from ethyl acetate/hexanes
  5. customdried under house vacuum
  6. additionThe solids were then added to THF (200 ml)
  7. customNext, the crude reaction
  8. custompurified by silica gel chromatography (DCM to 10% MeOH/DCM over 30 min)
  9. dissolutionThe isolated pure amide was redissolved in 1,4-dioxane (10 ml)
  10. temperaturethe reaction was heated in the microwave at 120° C. for 20 min
  11. custompurified by silica gel chromatography (DCM to 10% MeOH/DCM)

출처 및 근거

ORD 기록
ord-a47f55879b854f40b20d90a5b98e143c
출처 데이터셋
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07981903B2

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