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Acetic Acid → N-{4-[4-methoxy-5-(2-methoxy-phenoxy)-6-(5-methyl-pyridine-2-sulfonylamino)-pyrimidin-2-yl]-pyridin-2-ylmethyl}-acetamide

HRID 1066512
ノート
印刷プレビュー

反応式

HRID 1066512 の反応式
[C:1]([OH:4])(=O)[CH3:2].CN1CCOCC1.ClC1N=C(OC)N=C(OC)N=1.Cl.[NH2:24][CH2:25][C:26]1[CH:31]=[C:30]([C:32]2[N:37]=[C:36]([NH:38][S:39]([C:42]3[CH:47]=[CH:46][C:45]([CH3:48])=[CH:44][N:43]=3)(=[O:41])=[O:40])[C:35]([O:49][C:50]3[CH:55]=[CH:54][CH:53]=[CH:52][C:51]=3[O:56][CH3:57])=[C:34]([O:58][CH3:59])[N:33]=2)[CH:29]=[CH:28][N:27]=1>CN(C=O)C>[CH3:59][O:58][C:34]1[C:35]([O:49][C:50]2[CH:55]=[CH:54][CH:53]=[CH:52][C:51]=2[O:56][CH3:57])=[C:36]([NH:38][S:39]([C:42]2[CH:47]=[CH:46][C:45]([CH3:48])=[CH:44][N:43]=2)(=[O:41])=[O:40])[N:37]=[C:32]([C:30]2[CH:29]=[CH:28][N:27]=[C:26]([CH2:25][NH:24][C:1](=[O:4])[CH3:2])[CH:31]=2)[N:33]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 176Acetic AcidHCID 79724-MethylmorpholineHCID 184502-Chloro-4,6-dimethoxy-1,3,5-triazineHCID 867569945-Methyl-pyridine-2-sulfonic acid [2-(2-aminomethyl-pyridin-4-yl)-6-methoxy-5-(2-methoxy-phenoxy)-pyrimidin-4-yl]-amide hydrochloride

生成物 1

HCID 21200272N-{4-[4-methoxy-5-(2-methoxy-phenoxy)-6-(5-methyl-pyridine-2-sulfonylamino)-pyrimidin-2-yl]-pyridin-2-ylmethyl}-acetamide

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 6.6 mg of acetic acid and 22.3 mg of 4-methylmorpholin in DMF (5 ml) were added under ice-cooling 22.3 g of 2-Chloro-4,6-dimethoxy-1,3,5,-triazine and the solution was then stirred for 90 minutes at RT. Then 60 mg of 5-methyl-pyridine-2-sulfonic acid [2-(2-aminomethyl-pyridin-4-yl)-6-methoxy-5-(2-methoxy-phenoxy)-pyrimidin-4-yl]-amide hydrochloride were added and stirring was continued for 12 h at RT. The mixture was partitioned between cold diluted HCl and EtOAc. The layers were separated the organic layer washed with water, dried over Na2SO4 and the solvent removed in vacuo to give N-{4-[4-methoxy-5-(2-methoxy-phenoxy)-6-(5-methyl-pyridine-2-sulfonylamino)-pyrimidin-2-yl]-pyridin-2-ylmethyl}-acetamide as a light yellow crystalline solid. ISN mass spectrum, m/e 549.1 (M−1 calculated for C26H26N6O6S: 549).

後処理

  1. stirringstirring
  2. waitwas continued for 12 h at RT
  3. customThe mixture was partitioned between cold diluted HCl and EtOAc
  4. customThe layers were separated the organic layer
  5. washwashed with water
  6. dry with materialdried over Na2SO4
  7. customthe solvent removed in vacuo

出典と根拠

ORDレコード
ord-e826e54149934c529d51c5cc1b8b20c4
出典データセット
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06242601B1

反応ノート

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