Dimethylamine → HCID 178508306、化合物

HRID 750538ノート

反応式

HRID 750538 の反応式
[NH2:1][C:2]1[N:3]=[C:4]([C:28]2[O:29][CH:30]=[CH:31][CH:32]=2)[C:5]2[N:10]=[N:9][N:8]([CH2:11][C:12]3[CH:27]=[CH:26][C:15]4[N:16](C(OC(C)(C)C)=O)[N:17]=[N:18][C:14]=4[CH:13]=3)[C:6]=2[N:7]=1.C1COCC1.CNC>CO>[NH:16]1[C:15]2[CH:26]=[CH:27][C:12]([CH2:11][N:8]3[C:6]4[N:7]=[C:2]([NH2:1])[N:3]=[C:4]([C:28]5[O:29][CH:30]=[CH:31][CH:32]=5)[C:5]=4[N:10]=[N:9]3)=[CH:13][C:14]=2[N:18]=[N:17]1

参加物

5

反応物 3

HCID 674DimethylamineHCID 8028TetrahydrofuranHCID 21874651HCID 21874651、化合物

生成物 1

HCID 178508306HCID 178508306、化合物収率 30%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of tert-butyl 5-(5-amino-7-(2-furyl)-3H-triazolo[4,5-d]pyrimidin-3-yl)methyl-1H-benzotriazol-1-carboxylate (as a mixture with the 6-substituted regioisomer) (135 mg, 0.31 mmol) in MeOH (5 mL) and THF (5 mL was treated with 40% aqueous dimethylamine (0.176 mL, 1.56 mmol), refluxed for 25 min, concentrated in vacuo and the resulting solid triturated with ether, filtered, triturated with MeOH, filtered and dried to give the title compound (31 mg, 30%) as a yellow solid.

後処理

  1. temperaturerefluxed for 25 min
  2. concentrationconcentrated in vacuo
  3. customthe resulting solid triturated with ether
  4. filtrationfiltered
  5. customtriturated with MeOH
  6. filtrationfiltered
  7. customdried

出典と根拠

ORDレコード
ord-091dab5286404a9dbf4abfa80a6b0b8f
出典データセット
uspto-grants-2008_07
特許番号
US07405219B2

反応ノート

読み込み中…