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Phosgene → HCID 54545133, 화합물

HRID 2287035
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HRID 2287035 반응식
[C:1](Cl)(Cl)=[O:2].[Cl:5][C:6]1[CH:7]=[C:8]([CH:18]=[C:19]([Cl:21])[CH:20]=1)[O:9][CH:10]([C:12]1[S:16][C:15]([NH2:17])=[N:14][N:13]=1)[CH3:11]>C(OCC)(=O)C>[Cl:5][C:6]1[CH:7]=[C:8]([CH:18]=[C:19]([Cl:21])[CH:20]=1)[O:9][CH:10]([C:12]1[S:16][C:15]([N:17]=[C:1]=[O:2])=[N:14][N:13]=1)[CH3:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6371Phosgene3회HCID 23460870HCID 23460870, 화합물

생성물 1

HCID 54545133HCID 54545133, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매3회

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 rotameter was charged with 50 milliliters of ethyl acetate saturated with phosgene at 20° C. (approximately 0.5 mole of phosgene). An additional 50 milliliters of ethylacetate was added, and 7.9 grams of 5-[1-(3,5-dichorophenoxy)ethyl]-2-amino-1,3,4-thiadiazole, (prepared above) in 30 milliliters of ethyl acetate was added. The resulting solution was stirred for 64 hours, and then purged with nitrogen until no COCl2 was detected. The solution was filtered and then topped at 70° C. in a roto-vac to form 10.0 grams of a viscous yellow oil of 5-[1-(3,5-dichlorophenoxy)ethyl]-1,3,4-thiadiazol-2-yl isocyanate dimer.

후처리

  1. customA 500 milliliter, 3-neck flask equipped with a magnetic stirrer
  2. additionwas added
  3. custompurged with nitrogen until no COCl2
  4. filtrationThe solution was filtered
  5. customtopped at 70° C. in a roto-vac

출처 및 근거

ORD 기록
ord-ea7e67af10f84700b65126bd94a4f45e
출처 데이터셋
uspto-grants-1981_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04268675

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