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Dichloromethane → HCID 178504155, 화합물

HRID 328599
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HRID 328599 반응식
[CH3:1][S:2](=[N:7][S:8]([C:11]1[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][CH:12]=1)(=[O:10])=[O:9])C(=O)SC.S(Cl)(Cl)(=O)=O.[Cl:23][CH2:24][Cl:25]>>[Cl:17][C:14]1[CH:13]=[CH:12][C:11]([S:8]([N:7]=[SH:2]([CH3:1])=[C:24]([Cl:25])[Cl:23])(=[O:10])=[O:9])=[CH:16][CH:15]=1
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참가 물질

4

반응물 3

HCID 6344DichloromethaneHCID 24648Sulfuryl chlorideHCID 131710711HCID 131710711, 화합물

생성물 1

HCID 178504155HCID 178504155, 화합물

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온도
35 °C

실험 절차

The N-(4-chlorophenylsulphonyl)-iminodithiocarbonic acid-S,S-dimethyl ester (1000 g) obtained in the manner described is suspended in 1000 ml of dichloromethane, and 290 ml of sulphonyl chloride (3.6 moles) is added dropwise to the suspension, whereupon a yellow solution is obtained with generation of SO2. This solution is heated for about 2 hours at a temperature of 35° C. The solvent as well as the formed methanesulphonyl chloride and unreacted sulphonyl chloride is distilled off in a Rotovap, and the crystallised residue is taken up in hexane. After filtration with suction there is obtained N-(4-chlorophenysulphonyl)-S-methyl-iminothiocarbonic acid chloride: m.p. 86°-89° C.

후처리

  1. customis obtained with generation of SO2
  2. distillationThe solvent as well as the formed methanesulphonyl chloride and unreacted sulphonyl chloride is distilled off in a Rotovap
  3. filtrationAfter filtration with suction

출처 및 근거

ORD 기록
ord-465efdd7bfd443e29256bd0f5033305e
출처 데이터셋
uspto-grants-1977_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04017638

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