Dimethylamine → HCID 178508306、化合物

HRID 733012ノート

反応式

HRID 733012 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-ef1b162935b34b19b770ebbe781a7e63
出典データセット
uspto-grants-2009_09
特許番号
US07589097B2

反応ノート

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