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Trifluoroacetic acid → N-[4-(2-Amino-9-(3-azidopropyl)-purine-6-yloxymethyl)-benzyl]-2,2,2-trifluoro-acetamide

HRID 1695086
ノート
印刷プレビュー

反応式

HRID 1695086 の反応式
[F:1][C:2]([F:16])([F:15])[C:3]([NH:5][CH2:6][C:7]1[CH:12]=[CH:11][C:10]([CH2:13][OH:14])=[CH:9][CH:8]=1)=[O:4].[H-].[Na+].[N:19]([CH2:22][CH2:23][CH2:24][N:25]1[CH:33]=[N:32][C:31]2[C:26]1=[N:27][C:28]([NH2:35])=[N:29][C:30]=2Cl)=[N+:20]=[N-:21].FC(F)(F)C(O)=O>CC(N(C)C)=O.O>[NH2:35][C:28]1[N:27]=[C:26]2[C:31]([N:32]=[CH:33][N:25]2[CH2:24][CH2:23][CH2:22][N:19]=[N+:20]=[N-:21])=[C:30]([O:14][CH2:13][C:10]2[CH:11]=[CH:12][C:7]([CH2:6][NH:5][C:3](=[O:4])[C:2]([F:15])([F:16])[F:1])=[CH:8][CH:9]=2)[N:29]=1
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 6422Trifluoroacetic acidHCID 24758Sodium hydrideHCID 15852209N-(4-Hydroxymethylbenzyl)trifluoroacetamideHCID 86067829N9-(3-Azidopropyl)-2-amino-6-chloropurine

生成物 1

HCID 58989129N-[4-(2-Amino-9-(3-azidopropyl)-purine-6-yloxymethyl)-benzyl]-2,2,2-trifluoro-acetamide

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 31374Dimethylacetamide溶媒

反応条件

温度
90 °C

実験手順

2,2,2-Trifluoro-N-(4-hydroxymethyl-benzyl)-acetamide (138 mg, 0.59 mmol) is dissolved in 3 mL dry dimethylacetamide under argon atmosphere, and (31 mg, 1.31 mmol) NaH is added. N9-(3-Azidopropyl)-2-amino-6-chloropurine (22, 100 mg, 0.39 mmol) is added and the solution heated to 90° C. for 16 h. After cooling to room temperature, the mixture is poured into 80 mL of water and the pH is adjusted to 6 with trifluoroacetic acid. The aqueous phase is extracted with CH2Cl2 and ethyl acetate. The organic phases are washed with water and brine, dried over MgSO4 and the solvent is evaporated. The crude product is dissolved in methanol, adsorbed on SiO2 (150 mg) and purified by flash column chromatography with dichloromethane:methanol (95:5). Yield: 151 mg (0.0336 mmol, 85%). 1H-NMR (400 MHz, DMSO-d6): δ=10.00 (t, J=5.8, 1H, CF3CONH), 7.90 (s, 1H, H-8), 7.49, (d, J=8.1, 2H, ArH), 7.28 (d, J=8.1, 2H, ArH), 6.47 (s br, 2H, NH2), 5.46 (s, 2H, OCH2), 4.38 (d, J=5.8, 2H, CH2NH), 4.06 (t, J=6.5, 2H, CH2), 3.36 (t, J=6.5, 2H, CH2), 2.00 (m, 2H, CH2) ppm. MS (ESI) m/z 450.0 [M+H]+.

後処理

  1. temperatureAfter cooling to room temperature
  2. extractionThe aqueous phase is extracted with CH2Cl2 and ethyl acetate
  3. washThe organic phases are washed with water and brine
  4. dry with materialdried over MgSO4
  5. customthe solvent is evaporated
  6. dissolutionThe crude product is dissolved in methanol
  7. custompurified by flash column chromatography with dichloromethane:methanol (95:5)

出典と根拠

ORDレコード
ord-0311eb9be0694e11a1c56e888b4c833f
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08163479B2

反応ノート

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