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

HRID 224597

반응식

HRID 224597 반응식
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]

참가 물질

8

반응물 6

HCID 313Hydrochloric AcidHCID 6577Chloroacetyl chlorideHCID 14798Sodium HydroxideHCID 516892Sodium BicarbonateHCID 178419078HCID 178419078, 화합물HCID 178526132HCID 178526132, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-1e802a9b9e5f46c99de6fd672afb14bd
출처 데이터셋
uspto-grants-1980_11
특허 번호
US04233310

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