Acetic Acid → HCID 86651251、化合物

HRID 538187

反応式

HRID 538187 の反応式
[Br:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[C:4]([Br:9])[C:3]=1[NH:10][C:11]([NH2:13])=S.[OH-].[K+].O.O.O.C([O-])(=O)C.[Pb+2].C([O-])(=O)C.C(O)(=O)C>O>[Br:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[C:4]([Br:9])[C:3]=1[NH:10][C:11]#[N:13]

参加物

6

反応物 4

HCID 176Acetic AcidHCID 14797Potassium HydroxideHCID 22456Lead diacetate trihydrateHCID 86651250(2,6-Dibromo-4-fluoro-phenyl)-thiourea

生成物 1

HCID 86651251HCID 86651251、化合物収率 63%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

A solution of (2,6-dibromo-4-fluoro-phenyl)-thiourea (0.300 g, 0.920 mmol) and 1M aq. KOH (7.23 mL) was heated to 100° C. Lead (II) acetate trihydrate (0.400 g, 1.05 mmol) in water (2 mL) was then added. The mixture was heated at 100° C. for another 10 minutes while a precipitate was observed. The mixture was cooled to 0° C. and filtered to provide a clear colorless solution. The filtrate was acidified to pH 5 with acetic acid. The precipitate was collected by filtration to yield titled compound (0.170 g, 63%). 1H NMR (400 MHz, DMSO-d6): 7.80-7.78 (m, 2H).

後処理

  1. temperatureThe mixture was cooled to 0° C.
  2. filtrationfiltered
  3. customto provide a clear colorless solution
  4. filtrationThe precipitate was collected by filtration

出典と根拠

ORDレコード
ord-cff54d57aac4440f935a65ca99714d38
出典データセット
uspto-grants-2014_10
特許番号
US08865713B2

関連ノート

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