Triethylamine → 3-Amino-2-Benzyl-5-Methoxy-2H-1,2,4,6-thiatriazine-1,1-dioxide

HRID 1252027ノート

反応式

HRID 1252027 の反応式
[CH2:1]([NH:8][S:9](Cl)(=[O:11])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:13]([NH:17][C:18](=[NH:21])[O:19][CH3:20])(OC)=O.C([N:24](CC)CC)C>C1COCC1>[NH2:24][C:13]1[N:8]([CH2:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[S:9](=[O:11])(=[O:10])[N:21]=[C:18]([O:19][CH3:20])[N:17]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 13529095Benzylsulfamyl chlorideHCID 137319931Methyl N-(iminomethoxymethyl)carbamate

生成物 1

HCID 201409183-Amino-2-Benzyl-5-Methoxy-2H-1,2,4,6-thiatriazine-1,1-dioxide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of benzylsulfamoyl chloride (168 g) in anhydrous THF (300 ml) is added dropwise to a stirred solution of N-carbomethoxy-O-methylisourea (107 g) and triethylamine (90 g) in anhydrous THF (800 ml) under nitrogen at -70° C. The resulting suspension is warmed to RT, filtered and the filtrate evaporated in vacuo. The residue is partitioned between methylene chloride and 0.5N aqueous HCl. The organic layer is dried, filtered, and concentrated in vacuo affording the desired product as an oil.

後処理

  1. filtrationfiltered
  2. customthe filtrate evaporated in vacuo
  3. customThe residue is partitioned between methylene chloride and 0.5N aqueous HCl
  4. customThe organic layer is dried
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-62b52b96d75b476896011517204416ba
出典データセット
uspto-grants-1988_05
特許番号
US04742055

反応ノート

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