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Diethyl Ether → Triethylammonium 6-propylpyrid-2-yldithiocarbamate

HRID 1862967
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인쇄 미리보기

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HRID 1862967 반응식
[C:1](=[S:3])=[S:2].[NH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([CH2:11][CH2:12][CH3:13])[N:6]=1.[CH2:14](OCC)[CH3:15]>C(#N)C.C(N(CC)CC)C>[CH2:11]([C:7]1[N:6]=[C:5]([NH:4][C:1](=[S:3])[S-:2])[CH:10]=[CH:9][CH:8]=1)[CH2:12][CH3:13].[CH2:14]([NH+:6]([CH2:5][CH3:10])[CH2:7][CH3:11])[CH3:15]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 3283Diethyl EtherHCID 6348Carbon DisulfideHCID 30163096-Propylpyridin-2-amine

생성물 1

HCID 20393053Triethylammonium 6-propylpyrid-2-yldithiocarbamate

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 8471Triethylamine용매

반응 조건

온도
20 °C

실험 절차

A solution of carbon disulphide (20 cc) in anhydrous acetonitrile (23 cc) is added, at 20° C., to a solution of 2-amino-6-propylpyridine (34.0 g) in anhydrous triethylamine (69 cc). After stirring of the mixture for 20 hours at 20° C., anhydrous diethyl ether (800 cc) is added. After cooling for 1 hour at 2° C., the resulting crystals are filtered off, washed three times with anhydrous diethyl ether (total 300 cc) and dried under reduced pressure (20 mm Hg) at 20° C. Triethylammonium 6-propylpyrid-2-yldithiocarbamate (50.3 g), melting at about 98° C., is obtained.

후처리

  1. temperatureAfter cooling for 1 hour at 2° C.
  2. filtrationthe resulting crystals are filtered off
  3. washwashed three times with anhydrous diethyl ether (total 300 cc)
  4. customdried under reduced pressure (20 mm Hg) at 20° C

출처 및 근거

ORD 기록
ord-b8869700fa1d4d5f804a71551e0503c4
출처 데이터셋
uspto-grants-1979_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04167571

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