Thiophosgene → 4-Ethoxycarbonyl-1-piperazinylthiocarbonyl chloride

HRID 1462334노트

반응식

HRID 1462334 반응식
[C:1]([Cl:4])(Cl)=[S:2].[CH2:5]([O:7][C:8]([N:10]1[CH2:15][CH2:14][N:13]([Si](C)(C)C)[CH2:12][CH2:11]1)=[O:9])[CH3:6]>C(OCC)C>[CH2:5]([O:7][C:8]([N:10]1[CH2:11][CH2:12][N:13]([C:1]([Cl:4])=[S:2])[CH2:14][CH2:15]1)=[O:9])[CH3:6]

참가 물질

4

반응물 2

HCID 10040ThiophosgeneHCID 133449251-Ethoxycarbonyl-4-trimethylsilylpiperazine

생성물 1

HCID 133449264-Ethoxycarbonyl-1-piperazinylthiocarbonyl chloride

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

To a solution of 4.66 ml of 85% thiophosgene in 200 ml of ethyl ether, cooled to -76° was added, while stirring and under nitrogen, a solution of 7 g of 1-ethoxycarbonyl-4-trimethylsilylpiperazine in 35 ml of ethyl ether over a period of 20 minutes. The mixture was allowed to warm up to room temperature overnight. The suspension was filtered and the filtrate was evaporated to dryness. The residue was crystallized from methylene chloride-hexane to give 4-ethoxycarbonyl-1-piperazinylthiocarbonyl chloride, m.p. 107°-111°.

후처리

  1. additionwas added
  2. filtrationThe suspension was filtered
  3. customthe filtrate was evaporated to dryness
  4. customThe residue was crystallized from methylene chloride-hexane

출처 및 근거

ORD 기록
ord-74158b3790fc4545a26d3fce5ab905f5
출처 데이터셋
uspto-grants-1984_07
특허 번호
US04460508

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