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Formaldehyde → 2-Cyano-4-[2-(1-methylpiperidin-4-yl)ethoxy]-6-[(spiro[2.5]oct-6-ylmethyl)amino]pyrimidine-5-carboxylic acid benzylamide

HRID 645518
ノート
印刷プレビュー

反応式

HRID 645518 の反応式
[CH2:1]([NH:8][C:9]([C:11]1[C:12]([O:29][CH2:30][CH2:31][CH:32]2[CH2:37][CH2:36][NH:35][CH2:34][CH2:33]2)=[N:13][C:14]([C:27]#[N:28])=[N:15][C:16]=1[NH:17][CH2:18][CH:19]1[CH2:26][CH2:25][C:22]2([CH2:24][CH2:23]2)[CH2:21][CH2:20]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C=O.[BH3-][C:41]#N.[Na+]>C1COCC1>[CH2:1]([NH:8][C:9]([C:11]1[C:12]([O:29][CH2:30][CH2:31][CH:32]2[CH2:37][CH2:36][N:35]([CH3:41])[CH2:34][CH2:33]2)=[N:13][C:14]([C:27]#[N:28])=[N:15][C:16]=1[NH:17][CH2:18][CH:19]1[CH2:20][CH2:21][C:22]2([CH2:23][CH2:24]2)[CH2:25][CH2:26]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 712FormaldehydeHCID 5003444Sodium cyanoborohydrideHCID 68708606HCID 68708606、化合物

生成物 1

HCID 445873662-Cyano-4-[2-(1-methylpiperidin-4-yl)ethoxy]-6-[(spiro[2.5]oct-6-ylmethyl)amino]pyrimidine-5-carboxylic acid benzylamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a solution of 2-cyano-4-(2-piperidin-4-yl-ethoxy)-6-[(spiro[2.5]oct-6-ylmethyl)amino]-pyrimidine-5-carboxylic acid benzylamide (0.19 mmol) in THF (2 mL) is added formaldehyde solution (100 μL), and the resulting solution is stirred for 0.5 h at room temperature. After cooled to 0° C., 1 M NaBH3CN solution in THF is added dropwise, and the reaction mixture is stirred for 2 h at room temperature. The reaction is quenched by the addition of H2O, and extracted twice with AcOEt. The organic layer is dried over Na2SO4, filtered, and concentrated. The residue is purified by silica gel column to give 2-cyano-4-[2-(1-methylpiperidin-4-yl)ethoxy]-6-[(spiro[2.5]oct-6-ylmethyl)amino]pyrimidine-5-carboxylic acid benzylamide as a colorless oil; 1H-NMR (CDCl3), δ 0.17-0.30 (4H, m), 0.89-0.94 (2H, m), 1.14-1.29 (3H, m), 1.40-1.50 (2H, m), 1.58-1.78 (9H, m), 1.95-2.01 (3H, m), 2.38 (3H, s), 2.95-2.98 (2H, m), 3.42 (2H, t), 4.46 (2H, t), 4.56 (2H, d), 7.31-7.39 (5H, m), 8.13 (1H, t), 10.16 (1H, t).

後処理

  1. temperatureAfter cooled to 0° C.
  2. stirringthe reaction mixture is stirred for 2 h at room temperature
  3. customThe reaction is quenched by the addition of H2O
  4. extractionextracted twice with AcOEt
  5. dry with materialThe organic layer is dried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe residue is purified by silica gel column

出典と根拠

ORDレコード
ord-51b0533e64184cd6a15288601653e68c
出典データセット
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07704996B2

反応ノート

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