Hydrochloric Acid → HCID 178425509、化合物

HRID 637937ノート

反応式

HRID 637937 の反応式
C(O)(=O)C[SH:3].[H-].[Na+].Cl[C:9]1[N:14]=[C:13]([Cl:15])[N:12]=[C:11]([NH:16][C:17]2[CH:22]=[CH:21][CH:20]=[C:19]([CH3:23])[C:18]=2[CH3:24])[N:10]=1.Cl.[CH2:26]([O:28]CC)[CH3:27]>CN(P(N(C)C)(N(C)C)=O)C>[Cl:15][C:13]1[N:12]=[C:11]([NH:16][C:17]2[CH:22]=[CH:21][CH:20]=[C:19]([CH3:23])[C:18]=2[CH3:24])[N:10]=[C:9]([CH2:27][C:26]([OH:28])=[S:3])[N:14]=1

参加物

7

反応物 5

HCID 313Hydrochloric AcidHCID 1133Thioglycolic AcidHCID 3283Diethyl EtherHCID 24758Sodium hydrideHCID 134137564,6-Dichloro-N-(2,3-dimethylphenyl)-1,3,5-triazin-2-amine

生成物 1

HCID 178425509HCID 178425509、化合物

試薬・触媒・溶媒 1

HCID 12679Hexamethylphosphoramide溶媒

実験手順

To a solution of thioglycolic acid (0.076 ml) in hexamethylphosphortriamide (2 ml), 100% sodium hydride (46 mg) is added, at room temperature, stirring for 15'. Then 2,4-dichloro-6-(2,3-xylidino)-1,3,5-triazine (0.26 g) in hexamethylphosphorotriamide (1.5 ml) is added, stirring for 30' more. The reaction mixture is then diluted with ethyl ether (15 ml), added with 10% HCl (7 ml) and stirred for 10'. The orgaic phase is separated, washed with water to neutrality and dried over Na2SO4. By evaporation of the solvent an oil (0.24 g) is obtained which crystallizes from ethyl acetate/hexane. Yield: 0.18 g of the title compound (V, 43).

後処理

  1. stirringstirring for 30' more
  2. stirringstirred for 10'
  3. customThe orgaic phase is separated
  4. washwashed with water to neutrality
  5. dry with materialdried over Na2SO4
  6. customBy evaporation of the solvent an oil (0.24 g)
  7. customis obtained which
  8. customcrystallizes from ethyl acetate/hexane

出典と根拠

ORDレコード
ord-c33c9b0b46c64ff68254e4591ee658f3
出典データセット
uspto-grants-1985_12
特許番号
US04559345

反応ノート

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