Thiophosgene → 4-Ethoxycarbonyl-1-piperazinylthiocarbonyl chloride

HRID 1462445노트

반응식

HRID 1462445 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° is 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 is allowed to warm up to room temperature overnight. The suspension is filtered and the filtrate is evaporated to dryness. The residue is crystallized from methylene chloridehexane to give 4-ethoxycarbonyl-1-piperazinylthiocarbonyl chloride, m.p. 107°-111°.

후처리

  1. additionis added
  2. filtrationThe suspension is filtered
  3. customthe filtrate is evaporated to dryness
  4. customThe residue is crystallized from methylene chloridehexane

출처 및 근거

ORD 기록
ord-cb570bf3d6be410db649bcca16b3a93c
출처 데이터셋
uspto-grants-1984_07
특허 번호
US04460587

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