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4-Methylmorpholine → 4-(3-(4-(Dimethylamino)benzamido)-2-fluorophenyl)-7-morpholino-9H-pyrido[3,4-b]indole-1-carboxamide

HRID 2361357
ノート
印刷プレビュー

反応式

HRID 2361357 の反応式
[CH3:1][N:2]([CH3:41])[C:3]1[CH:40]=[CH:39][C:6]([C:7]([NH:9][C:10]2[C:11]([F:38])=[C:12]([C:16]3[C:28]4[C:27]5[C:22](=[CH:23][C:24]([N:29]6[CH2:34][CH2:33][O:32][CH2:31][CH2:30]6)=[CH:25][CH:26]=5)[NH:21][C:20]=4[C:19]([C:35]([OH:37])=O)=[N:18][CH:17]=3)[CH:13]=[CH:14][CH:15]=2)=[O:8])=[CH:5][CH:4]=1.[Cl-].[NH4+].C([N:47](CC)C(C)C)(C)C.F[P-](F)(F)(F)(F)F.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1.CN1CCOCC1>CN(C=O)C.CO>[CH3:41][N:2]([CH3:1])[C:3]1[CH:4]=[CH:5][C:6]([C:7]([NH:9][C:10]2[C:11]([F:38])=[C:12]([C:16]3[C:28]4[C:27]5[C:22](=[CH:23][C:24]([N:29]6[CH2:34][CH2:33][O:32][CH2:31][CH2:30]6)=[CH:25][CH:26]=5)[NH:21][C:20]=4[C:19]([C:35]([NH2:47])=[O:37])=[N:18][CH:17]=3)[CH:13]=[CH:14][CH:15]=2)=[O:8])=[CH:39][CH:40]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 79724-MethylmorpholineHCID 25517Ammonium ChlorideHCID 81531DiisopropylethylamineHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 679950664-(3-(4-(Dimethylamino)benzamido)-2-fluorophenyl)-7-morpholino-9H-pyrido[3,4-b]indole-1-carboxylic acid

生成物 1

HCID 70651681
4-(3-(4-(Dimethylamino)benzamido)-2-fluorophenyl)-7-morpholino-9H-pyrido[3,4-b]indole-1-carboxamide
収率 23.2%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 4-(3-(4-(dimethylamino)benzamido)-2-fluorophenyl)-7-morpholino-9H-pyrido[3,4-b]indole-1-carboxylic acid (105 mg, 0.190 mmol), ammonium chloride (40.6 mg, 0.759 mmol), N,N-diisopropylethylamine (0.159 mL, 0.910 mmol), BOP (109 mg, 0.247 mmol), N-methylmorpholine (0.081 mL, 0.740 mmol) in DMF (0.5 mL) was stirred at room temperature for 1.5 hr. The mixture was diluted with MeOH (4 mL), divided into three portions, and purified by reverse phase HPLC. The correct fractions were concentrated under vacuum and basified with saturated NaHCO3 solution to pH 10. The precipitating product (24.7 mg, 0.044 mmol, 23.09% yield) was collected as a yellow solid by suction filtration and dried at 50° C. under vacuum. LCMS (M+H)+=553.32. 1H NMR (500 z, DMSO-d6) δ: 11.52 (s, 1H), 9.86 (s, 1H), 8.31 (s, 1H), 8.20 (s, 1H), 7.90 (d, J=9.0 Hz, 2H), 7.84 (m, 1H), 7.76 (s, 1H), 7.45-7.40 (m, 2H), 7.32 (d, J=8.0 Hz, 1H), 7.29 (d, J=2.0 Hz, 1H), 6.86 (dd, J1=9.0 Hz, J2=2.0 Hz, 1H), 6.77 (d, J=9.0 Hz, 2H), 3.79-3.77 (m, 4H), 3.22-3.19 (m, 4H), 2.51 (m, 6H).

後処理

  1. custompurified by reverse phase HPLC
  2. concentrationThe correct fractions were concentrated under vacuum

出典と根拠

ORDレコード
ord-bcde4d8ea73949598c33139e133bd1c1
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08685969B2

反応ノート

読み込み中…

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