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Methyl iodide → Methyl 5-[3-(4-{1-[(tert-butoxycarbonyl)amino]cyclobutyl}phenyl)-9H-imidazo[1,2-d]pyrido[2,3-b][1,4]benzodiazepin-2-yl]pyridine-2-carboxylate

HRID 1047053
ノート
印刷プレビュー

反応式

HRID 1047053 の反応式
Br[C:2]1[N:3]=[C:4]2[C:10]3[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=3[NH:8][C:7]3[N:15]=[CH:16][CH:17]=[CH:18][C:6]=3[N:5]2[C:19]=1[C:20]1[CH:25]=[CH:24][C:23]([C:26]2([NH:30][C:31](=[O:37])[O:32][C:33]([CH3:36])([CH3:35])[CH3:34])[CH2:29][CH2:28][CH2:27]2)=[CH:22][CH:21]=1.[CH3:38][O:39][C:40]([C:42]1[N:47]=[CH:46][C:45](B(O)O)=[CH:44][CH:43]=1)=[O:41].C([O-])([O-])=O.[Na+].[Na+].C(=O)([O-])[O-].[K+].[K+].IC>CN(C=O)C.CCOC(C)=O.CC(P(C(C)(C)C)C1C=CC(N(C)C)=CC=1)(C)C.CC(P(C(C)(C)C)C1C=CC(N(C)C)=CC=1)(C)C.Cl[Pd]Cl>[C:33]([O:32][C:31]([NH:30][C:26]1([C:23]2[CH:22]=[CH:21][C:20]([C:19]3[N:5]4[C:6]5[CH:18]=[CH:17][CH:16]=[N:15][C:7]=5[NH:8][C:9]5[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=5[C:4]4=[N:3][C:2]=3[C:45]3[CH:44]=[CH:43][C:42]([C:40]([O:39][CH3:38])=[O:41])=[N:47][CH:46]=3)=[CH:25][CH:24]=2)[CH2:27][CH2:28][CH2:29]1)=[O:37])([CH3:35])([CH3:34])[CH3:36]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 6328Methyl iodideHCID 10340Sodium CarbonateHCID 11430Potassium CarbonateHCID 455881876-(Methoxycarbonyl)pyridine-3-boronic acidHCID 136331865tert-butyl {1-[4-(2-bromo-9H-imidazo[1,2-d]pyrido[2,3-b][1,4]benzodiazepin-3-yl)phenyl]cyclobutyl}carbamate

生成物 1

HCID 67503711
Methyl 5-[3-(4-{1-[(tert-butoxycarbonyl)amino]cyclobutyl}phenyl)-9H-imidazo[1,2-d]pyrido[2,3-b][1,4]benzodiazepin-2-yl]pyridine-2-carboxylate
収率 95%

試薬・触媒・溶媒 3

HCID 11714597Bis(di-tert-butyl(4-dimethylaminophenyl)phosphine)dichloropalladium(II)触媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of tert-butyl {1-[4-(2-bromo-9H-imidazo[1,2-d]pyrido[2,3-b][1,4]benzodiazepin-3-yl)phenyl]cyclobutyl}carbamate (50 mg, 0.090 mmol), [6-(methoxycarbonyl)pyridin-3-yl]boronic acid (32 mg, 0.18 mmol), bis (di-tert-butyl(4-dimethylaminophenyl)phosphine)dichloropalladium(II) (6 mg, 0.09 mmol), and 2M Na2CO3 aq. (0.090 mL, 0.18 mmol) in DMF (2.5 mL) was treated with microwave (160° C. for 1 hour). The reaction mixture was added potassium carbonate (30 mg, 0.22 mmol) and iodomethane (0.050 mL, 0.80 mmol) and stirred at r.t for 17 hours. The mixture was diluted with AcOEt, washed with water(×3), brine, dried over Na2SO4, then filtrated through Celite pad. The filtrate was concentrated and the residue was purified by preparative thin-layer chromatography (n-hexane/AcOEt=1:3) to afford the desired product (52 mg, 95%) as a pale yellow solid. 1HNMR (CDCl3) 400 MHz δ: 8.83 (d, J=2.3 Hz, 1H), 8.15 (dd, J=7.4 Hz and 1.7 Hz, 1H), 8.09 (d, J=8.0 Hz, 1H), 8.02 (d, J=4.0 Hz, 1H), 7.41 (d, J=8.0 Hz, 2H), 7.34 (td, J=7.4 Hz and 1.7 Hz, 1H), 7.19-7.17 (m, 3H), 6.96 (d, J=8.0 Hz, 1H), 6.80 (d, J=7.4 Hz, 1H), 6.60 (dd, J=8.0 Hz and 4.6 Hz, 1H), 6.26 (s, 1H), 5.14 (br s, 1H), 3.99 (s, 3H), 2.59-2.53 (m, 2H), 2.51-2.42 (m, 2H), 2.20-2.12 (m, 1H), 1.96-1.88 (m, 1H), 1.40 (br s, 9H). LCMS: 615 [M+H].

後処理

  1. additionwas treated with microwave (160° C. for 1 hour)
  2. washwashed with water(×3), brine
  3. dry with materialdried over Na2SO4
  4. filtrationfiltrated through Celite pad
  5. concentrationThe filtrate was concentrated
  6. customthe residue was purified by preparative thin-layer chromatography (n-hexane/AcOEt=1:3)

出典と根拠

ORDレコード
ord-2475118e31d249afbb84d86c1592162b
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08569331B2

反応ノート

読み込み中…

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