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Diazopropane → HCID 13517200, 화합물

HRID 1589132
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인쇄 미리보기

반응식

HRID 1589132 반응식
[N+:1](=[CH:3][CH2:4][CH3:5])=[N-].[Cl:6][C:7]1[CH:12]=[CH:11][C:10]([S:13][C:14]2[S:19][C:18](=[S:20])N[C:16](=[O:21])[N:15]=2)=[CH:9][CH:8]=1>CCOCC.O1CCCC1>[CH2:3]([N:1]1[C:16](=[O:21])[N:15]=[C:14]([S:13][C:10]2[CH:11]=[CH:12][C:7]([Cl:6])=[CH:8][CH:9]=2)[S:19][C:18]1=[S:20])[CH2:4][CH3:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 12224242DiazopropaneHCID 13517199HCID 13517199, 화합물

생성물 1

HCID 13517200HCID 13517200, 화합물수율 66.4%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 7.7 g of diazopropane in ether is added in portions to a solution of 28.8 g of 2,3-dihydro-6-(4-chlorophenylthio)-2-thioxo-4H-1,3,5-thiadiazin-4-one in 250 ml of tetrahydrofuran at 22° C. The solvent is distilled off, the residue is taken up in a small amount of methanol, and the precipitate is filtered off under suction, washed with methanol and dried. 21.9 g of 3-propyl-6-(4-chlorophenylthio)-2-thioxo-1,3,5-thiadiazin-4-one are obtained in the form of yellow crystals of melting point 151°-152° C.

후처리

  1. distillationThe solvent is distilled off
  2. filtrationthe precipitate is filtered off under suction
  3. washwashed with methanol
  4. customdried

출처 및 근거

ORD 기록
ord-e29193bfc1234094bf7741b8ee57c097
출처 데이터셋
uspto-grants-1986_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04568672

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