Ethanesulfonylchloride, 2-chloro- → 9-(6-Methoxynaphthalen-2-yl)-3,4-dihydropyrido[2,1-c][1,2,4]thiadiazine 2,2-dioxide

HRID 1622721ノート

反応式

HRID 1622721 の反応式
[H-].[Na+].Cl[CH2:4][CH2:5][S:6](Cl)(=[O:8])=[O:7].[CH3:10][O:11][C:12]1[CH:13]=[C:14]2[C:19](=[CH:20][CH:21]=1)[CH:18]=[C:17]([C:22]1[C:23]([NH2:28])=[N:24][CH:25]=[CH:26][CH:27]=1)[CH:16]=[CH:15]2>C1COCC1>[CH3:10][O:11][C:12]1[CH:13]=[C:14]2[C:19](=[CH:20][CH:21]=1)[CH:18]=[C:17]([C:22]1[C:23]3=[N:28][S:6](=[O:8])(=[O:7])[CH2:5][CH2:4][N:24]3[CH:25]=[CH:26][CH:27]=1)[CH:16]=[CH:15]2

参加物

5

反応物 3

HCID 15385Ethanesulfonylchloride, 2-chloro-HCID 24758Sodium hydrideHCID 655501443-(6-Methoxynaphthalen-2-yl)pyridin-2-amine

生成物 1

HCID 667483539-(6-Methoxynaphthalen-2-yl)-3,4-dihydropyrido[2,1-c][1,2,4]thiadiazine 2,2-dioxide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a suspension of NaH (60%, 951 mg) in THF (dry) (40 ml) was added 2-chloroethanesulfonyl chloride (1.50 ml) at 0° C. and the mixture was stirred for 5 min at the same temperature. A solution of 3-(6-methoxynaphthalen-2-yl)pyridin-2-amine (1190 mg) in THF (dry) (25 mL) was added at 0° C. and the mixture was stirred at room temperature overnight. The mixture was quenched with water. Water and EtOAc were added and the precipitates were collected, washed with water/EtOAc, dried in vacuo to give the title compound (835.3 mg). A part of this was recrystallized from MeCN-THF/IPE.

後処理

  1. stirringthe mixture was stirred at room temperature overnight
  2. customThe mixture was quenched with water
  3. additionWater and EtOAc were added
  4. customthe precipitates were collected
  5. washwashed with water/EtOAc
  6. customdried in vacuo

出典と根拠

ORDレコード
ord-225776dd93a2453d8f0f94cda54742bd
出典データセット
uspto-grants-2014_07
特許番号
US08778934B2

反応ノート

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