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Phosgene → HCID 13489817, 화합물

HRID 1980777
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HRID 1980777 반응식
C(N[C:6]([NH:8][S:9]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[C:18]1[O:22][N:21]=[CH:20][CH:19]=1)(=[O:11])=[O:10])=[O:7])CCC.C1N2CCN(CC2)C1.C(Cl)(Cl)=O>C1(C)C(C)=CC=CC=1>[O:22]1[C:18]([C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=2[S:9]([N:8]=[C:6]=[O:7])(=[O:11])=[O:10])=[CH:19][CH:20]=[N:21]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6371PhosgeneHCID 9237DabcoHCID 13489816HCID 13489816, 화합물

생성물 1

HCID 13489817HCID 13489817, 화합물

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

A suspension of 6 g of N-(butylaminocarbonyl)-2-(isoxazol-5-yl)benzenesulfonamide, prepared in Example 6, in 50 ml of xylene containing 0.2 g of DABCO was heated at 130°-135° C. while 1.6 ml of phosgene was added portionwise at a rate to maintain a reflux temperature of 130°-135° C. The mixture was refluxed for an additional 2 hours, cooled under nitrogen to room temperature, filtered, and the filtrate was concentrated to dryness in vacuo. A sample of the crude oily product displayed a characteristic sulfonyl isocyanate band in the IR at 2200 cm-1.

후처리

  1. additionwas added portionwise at a rate
  2. temperatureto maintain a reflux temperature of 130°-135° C
  3. temperatureThe mixture was refluxed for an additional 2 hours
  4. filtrationfiltered
  5. concentrationthe filtrate was concentrated to dryness in vacuo

출처 및 근거

ORD 기록
ord-59516195023c473fa7640187060a440e
출처 데이터셋
uspto-grants-1985_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04511392

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