Phosgene → HCID 53680789, 화합물

HRID 1414097노트

반응식

HRID 1414097 반응식
[C:1](Cl)(Cl)=[O:2].[CH3:5][C:6]1[CH:20]=[CH:19][C:9]([O:10][CH:11]([C:13]2[S:17][C:16]([NH2:18])=[N:15][N:14]=2)[CH3:12])=[CH:8][CH:7]=1>C(OC(=O)C)C>[CH3:5][C:6]1[CH:7]=[CH:8][C:9]([O:10][CH:11]([C:13]2[S:17][C:16]([N:18]=[C:1]=[O:2])=[N:15][N:14]=2)[CH3:12])=[CH:19][CH:20]=1

참가 물질

4

반응물 2

HCID 6371Phosgene3회HCID 17604534HCID 17604534, 화합물

생성물 1

HCID 53680789HCID 53680789, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

A 500 milliliter, 3-neck flask equipped with a magnetic stirrer, thermometer, dry ice condenser/drying tube and inlet from a phosgene (COCl2) tank via a calibrated rotometer was charged with 50 milliliters of ethylacetate which was saturated with phosgene at 20° C. (approximately 0.5 mole of phosgene) and cooled in an ice bath. An additional 50 milliliters of ethylacetate was added and then 4.8 grams of 5-[1-(4-methylphenoxy)ethyl]-2-amino-1,3,4-thiadiazole (prepared above) was added, the solution was stirred overnight and then filtered to remove a small amount of insoluble sediment. The clear solution was topped on a roto-vac at 70° C. to form 4.0 grams of a viscous orange oil of 5-[1-(4-methylphenoxy)ethyl]-1,3,4-thiadiazol-2-yl isocyanate dimer.

후처리

  1. customA 500 milliliter, 3-neck flask equipped with a magnetic stirrer
  2. temperaturecooled in an ice bath
  3. filtrationfiltered
  4. customto remove a small amount of insoluble sediment
  5. customwas topped on a roto-vac at 70° C.

출처 및 근거

ORD 기록
ord-0ae350497d684f18bc8fd475502b3f0f
출처 데이터셋
uspto-grants-1981_02
특허 번호
US04252961

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