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Methylamine → HCID 178485529、化合物

HRID 1014509
ノート
印刷プレビュー

反応式

HRID 1014509 の反応式
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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 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

生成物 1

HCID 178485529HCID 178485529、化合物収率 39%

試薬・触媒・溶媒

2
HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
65 °C

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-a47f55879b854f40b20d90a5b98e143c
出典データセット
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07981903B2

反応ノート

読み込み中…

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