Hydrochloric Acid → Benzenecarbothioic acid, sodium salt (1:1)

HRID 224597

反応式

HRID 224597 の反応式
N[C@H](C(O)=O)CC1N=CNC=1.C(=O)([O-])O.[Na+:16].ClCC(Cl)=O.[C:22]([OH:30])(=[S:29])[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1.[OH-].[Na+].Cl>O>[C:22]([O-:30])(=[S:29])[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1.[Na+:16]

参加物

8

反応物 6

HCID 313Hydrochloric AcidHCID 6577Chloroacetyl chlorideHCID 14798Sodium HydroxideHCID 516892Sodium BicarbonateHCID 178419078HCID 178419078、化合物HCID 178526132HCID 178526132、化合物

生成物 1

HCID 23688990Benzenecarbothioic acid, sodium salt (1:1)

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

155 g of L-histidine and 189 g of sodium hydrogen carbonate were dissolved in 1 liter of water and 124 g of chloroacetyl chloride was added dropwise to the resulting solution with stirring and ice-cooling. After allowing the reaction to proceed for 1 hour, an aqueous solution of sodium thiobenzoate which was prepared from 152 g of thiobenzoic acid and 220 ml of 5 N solution of sodium hydroxide solution, was added dropwise to the resulting solution and was kept standing overnight at room temperature to allow reaction. The resulting reation solution was acidified with hydrochloric acid with ice-cooling to precipitate crystals. The crystals were collected on the filter and washed with water. The product thus obtained weighed 140 g (42 percent of the theoretical amount). Recrystallization from water gave colorless needles, m.p. 176°-177° C.

後処理

  1. temperatureice-cooling
  2. customthe reaction
  3. additionwas added dropwise to the resulting solution
  4. waitwas kept standing overnight at room temperature
  5. customreaction
  6. temperaturecooling
  7. customto precipitate crystals
  8. customThe crystals were collected on the
  9. filtrationfilter
  10. washwashed with water
  11. customThe product thus obtained
  12. customRecrystallization from water
  13. customgave colorless needles, m.p. 176°-177° C.

出典と根拠

ORDレコード
ord-1e802a9b9e5f46c99de6fd672afb14bd
出典データセット
uspto-grants-1980_11
特許番号
US04233310

関連ノート

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