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(S)-1-(5-Bromopyrimidin-2-yl)-N-(2,4-dichlorobenzyl)pyrrolidin-3-amine → (S)-(2,4-Dichlorobenzyl)-[1-(5-methylpyrimidin-2-yl)-pyrrolidin-3-yl]-amine

HRID 252123
ノート
印刷プレビュー

反応式

HRID 252123 の反応式
[CH3:1][Al](C)C.Br[C:6]1[CH:7]=[N:8][C:9]([N:12]2[CH2:16][CH2:15][C@H:14]([NH:17][CH2:18][C:19]3[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][C:20]=3[Cl:26])[CH2:13]2)=[N:10][CH:11]=1>C1COCC1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[Cl:26][C:20]1[CH:21]=[C:22]([Cl:25])[CH:23]=[CH:24][C:19]=1[CH2:18][NH:17][C@H:14]1[CH2:15][CH2:16][N:12]([C:9]2[N:8]=[CH:7][C:6]([CH3:1])=[CH:11][N:10]=2)[CH2:13]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

5

反応物 2

HCID 11503055(S)-1-(5-Bromopyrimidin-2-yl)-N-(2,4-dichlorobenzyl)pyrrolidin-3-amineHCID 16682925Trimethylaluminum2 回

生成物 1

HCID 59860363(S)-(2,4-Dichlorobenzyl)-[1-(5-methylpyrimidin-2-yl)-pyrrolidin-3-yl]-amine

試薬・触媒・溶媒 2

HCID 9811564Bis(dibenzylideneacetone)palladium触媒2 回HCID 8028
Tetrahydrofuran
溶媒

反応条件

温度
65 °C

実験手順

Add trimethylaluminium (2 N in hexanes, 190 μL, 0.32 mmol) and tetrakis(triphenylphosphine)palladium (0) (26 mg, 0.022 mmol) to (S)-[1-(5-bromopyrimidin-2-yl)-pyrrolidin-3-yl]-(2,4-dichlorobenzyl)-amine in dry THF (1.5 mL) and heat at 65° C. for 2 h, then add extra trimethylaluminium (2 N in hexanes, 190 μL, 0.32 mmol) and tetrakis(triphenylphosphine)palladium (0) (26 mg, 0.022 mmol) and heat at 65° C. for 30 min and 48 h at room temperature. Add water and extract with chloroform. Combine the organic layers and wash with saturated aqueous sodium chloride, dry (magnesium sulfate), concentrate and dissolve the residue in methanol (2 mL) and deposit onto an SCX-2 cartridge; eluting with methanol, then with 2 N ammonia in methanol. Concentrate the ammonia washing and chromatograph the residue by preparative mass guided chromatography to give the title compound as a residue. Treatment of the residue essentially as described in Example 1 gives the title compound as its hydrochloride. 1H NMR (300 MHz, CDCl3) δ 8.16 (2H, s), 7.37 (2H, dd, J=5.09, 3.01 Hz), 7.21 (1H, dd, J=8.29, 2.07 Hz), 3.90 (2H, d, J=4.90 Hz), 3.68-3.83 (2H, m), 3.58 (1H, m), 3.39-3.51 (2H, m), 2.14-2.25 (1H, m), 2.12 (3H, s), 1.84-1.96 (1H, m), MS (ES): m/z=337 [M+].

後処理

  1. temperatureheat at 65° C. for 30 min and 48 h at room temperature
  2. extractionAdd water and extract with chloroform
  3. washwash with saturated aqueous sodium chloride
  4. dry with materialdry (magnesium sulfate)
  5. concentrationconcentrate
  6. dissolutiondissolve the residue in methanol (2 mL)
  7. washeluting with methanol
  8. concentrationConcentrate the ammonia washing and chromatograph the residue by preparative mass

出典と根拠

ORDレコード
ord-81f0f935cd304437802f8857533d7a82
出典データセット
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07868014B2

反応ノート

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