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Triethylamine → 1,3-Dithiolan-2-one, O-((((1,1-dimethylethyl)dithio)methylamino)carbonyl)oxime

HRID 224384
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HRID 224384 반응식
[N:1](=[C:3]1[S:7][CH2:6][CH2:5][S:4]1)[OH:2].[CH3:8][N:9]([S:13][S:14][C:15]([CH3:18])([CH3:17])[CH3:16])[C:10](F)=[O:11].C(N(CC)CC)C>O1CCOCC1>[CH3:8][N:9]([S:13][S:14][C:15]([CH3:18])([CH3:17])[CH3:16])[C:10]([O:2][N:1]=[C:3]1[S:7][CH2:6][CH2:5][S:4]1)=[O:11]
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 124040782-Oximino-1,3-dithiolaneHCID 20399612N-methyl-N-(tert-butylthiosulfenyl)carbamoyl fluoride

생성물 1

HCID 30596081,3-Dithiolan-2-one, O-((((1,1-dimethylethyl)dithio)methylamino)carbonyl)oxime

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

2-[[O-[N-Methyl-N-(tert-butylthiosulfenyl)carbamoyl]oximino]]-1,3-dithiolane was prepared according to the procedure described in Example I, by reacting 2.9 g (0.0214 m) of 2-oximino-1,3-dithiolane, 4.23 g (0.0214 m) of N-methyl-N-(tert-butylthiosulfenyl)carbamoyl fluoride and 2.17 g (0.0214 m) of triethylamine in 50 ml of dioxane. 2-[[O-[N-Methyl-N-tert-butylthiosulfenyl)carbamoyl]oximino]]-1,3-dithiolane crystallized from methylene chloride isopropyl ether to yield 4.0 g of a white solid. It was then recrystallized from ethyl acetate to yield a solid, m.p. 112°-114° C.

후처리

  1. custom2-[[O-[N-Methyl-N-tert-butylthiosulfenyl)carbamoyl]oximino]]-1,3-dithiolane crystallized from methylene chloride isopropyl ether

출처 및 근거

ORD 기록
ord-badd9a2a625a4508953c96755c87c88a
출처 데이터셋
uspto-grants-1980_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04232035

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