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Water → HCID 178519017, 화합물

HRID 1834190
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HRID 1834190 반응식
[C:1]([N:3]=[C:4]([S-:6])[S-:5])#[N:2].[K+].[K+].[OH2:9].[CH2:10](Cl)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1>CO>[OH:9][C:1]1[N:3]=[C:4]([S:6][CH2:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[S:5][N:2]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 7503Benzyl ChlorideHCID 83179Carbamodithioic acid, N-cyano-, potassium salt (1:2)

생성물 1

HCID 178519017HCID 178519017, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 194.4 of dipotassium N-cyano-dithioimidocarbonate, 150 ml of water, 1 liter of methanol and 126.7 g of benzyl chloride was stirred at room temperature for 1 hour and after filtering, methanol was evaporated from the filtrate 2.5 liters of water were added again to the residue and then 110 ml of 30% hydrogen peroxide were slowly added. The mixture was stirred for one half hour at 40° C and then 15 hours at 20° C. The mixture was acidified with hydrochloric acid and was vacuum filtered. The precipitate was crystallized from toluene to obtain 80 g of 3-hydroxy-5-benzylthio-1,2,4-thiadiazole melting at 125° C.

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후처리

  1. filtrationafter filtering
  2. custommethanol was evaporated from the filtrate 2.5 liters of water
  3. additionwere added again to the residue
  4. addition110 ml of 30% hydrogen peroxide were slowly added
  5. stirringThe mixture was stirred for one half hour at 40° C
  6. custom15 hours
  7. customat 20° C
  8. filtrationfiltered
  9. customThe precipitate was crystallized from toluene

출처 및 근거

ORD 기록
ord-afcb21ba4aed4286b842ceab9717180f
출처 데이터셋
uspto-grants-1978_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04069319

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