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Water → HCID 178519018, 화합물

HRID 1834193
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HRID 1834193 반응식
[Cl:1][C:2]1[CH:9]=[C:8]([Cl:10])[CH:7]=[CH:6][C:3]=1[CH2:4]Cl.[C:11]([N:13]=[C:14]([S-:16])[S-:15])#[N:12].[K+].[K+].[OH2:19]>CO>[OH:19][C:11]1[N:13]=[C:14]([S:16][CH2:4][C:3]2[CH:6]=[CH:7][C:8]([Cl:10])=[CH:9][C:2]=2[Cl:1])[S:15][N:12]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 72122,4-Dichlorobenzyl chlorideHCID 83179Carbamodithioic acid, N-cyano-, potassium salt (1:2)

생성물 1

HCID 178519018HCID 178519018, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
30 °C

실험 절차

72 g of 2,4-dichlorobenzyl chloride were added at 30° C to a mixture of 69.9 g of dipotassium N-cyanodithioimidocarbonate, 50 ml of water and 300 ml of methanol and the mixture was stirred at 30° C. for one-half hour. The methanol was evaporated under reduced pressure and 900 ml of water were added to the residue. 40 ml of 30% hydrogen peroxide were slowly added and the pH was kept basic by addition of potassium hydroxide. the mixture was stirred for 17 hours, was washed with ethyl acetate and was acidified with hydrochloric acid. The mixture was vacuum filtered and the precipitate was crystallized from toluene to obtain 32 g of 3-hydroxy-5-(2,4-dichlorobenzylthio)-1,2,4-thiadiazole melting at 134° C.

후처리

  1. customThe methanol was evaporated under reduced pressure and 900 ml of water
  2. additionwere added to the residue
  3. addition40 ml of 30% hydrogen peroxide were slowly added
  4. additionthe pH was kept basic by addition of potassium hydroxide
  5. stirringthe mixture was stirred for 17 hours
  6. washwas washed with ethyl acetate
  7. filtrationfiltered
  8. customthe precipitate was crystallized from toluene

출처 및 근거

ORD 기록
ord-c77b8abf7db44a2c8cfd9b45615cee19
출처 데이터셋
uspto-grants-1978_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04069319

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