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Methane → N-methyl-2-(pyrid-2-yl)-tetrahydrothiopyran-2-carbothioamide

HRID 1701891
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HRID 1701891 반응식
[CH3:1][NH2:2].[N:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]1([C:15]([S:17]C)=S)[CH2:14][CH2:13][CH2:12][CH2:11][S:10]1.C>C(O)C>[CH3:1][NH:2][C:15]([C:9]1([C:4]2[CH:5]=[CH:6][CH:7]=[CH:8][N:3]=2)[CH2:14][CH2:13][CH2:12][CH2:11][S:10]1)=[S:17]
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참가 물질

5

반응물 3

HCID 297MethaneHCID 6329MethylamineHCID 13043960Methyl 2-(pyrid-2-yl)-tetrahydrothiopyran-2-carbodithioate

생성물 1

HCID 13139530N-methyl-2-(pyrid-2-yl)-tetrahydrothiopyran-2-carbothioamide

시약·촉매·용매 1

HCID 702Ethanol용매3회

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온도
20 °C

실험 절차

A 33% (weight/volume) solution of methylamine in ethanol (7.5 cc) is added dropwise and in the course of 15 minutes to a solution of methyl 2-(pyrid-2-yl)-tetrahydrothiopyran-2-carbodithioate (9 g) in ethanol (60 cc), kept at a temperature of about 20° C. The solution is then stirred for 16 hours at a temperature of about 20° C. The resulting crystals are filtered off, washed twice with ethanol (20 cc in total) and dried under reduced pressure (20 mm Hg; 2.7 kPa) at a temperature of about 20° C. A crystalline crude product (7.8 g) is thus obtained, which is redissolved in boiling ethanol (96 cc); decolourising charcoal (0.4 g) is added to the solution thus obtained, which is filtered hot, and the filtrate is then cooled for 30 minutes at 0° C. The resulting crystals are filtered off, washed twice with ethanol (20 cc in total) and dried under reduced pressure (1 mm Hg; 0.13 kPa) at 45° C. N-Methyl-2-(pyrid-2-yl)-tetrahydrothiopyran-2-carbothioamide (6.3 g), melting at 153° C., is thus obtained.

후처리

  1. customkept at a temperature of about 20° C
  2. filtrationThe resulting crystals are filtered off
  3. washwashed twice with ethanol (20 cc in total)
  4. customdried under reduced pressure (20 mm Hg; 2.7 kPa) at a temperature of about 20° C
  5. customA crystalline crude product (7.8 g) is thus obtained
  6. dissolutionwhich is redissolved
  7. customthus obtained
  8. filtrationwhich is filtered hot
  9. temperaturethe filtrate is then cooled for 30 minutes at 0° C
  10. filtrationThe resulting crystals are filtered off
  11. washwashed twice with ethanol (20 cc in total)
  12. customdried under reduced pressure (1 mm Hg; 0.13 kPa) at 45° C

출처 및 근거

ORD 기록
ord-0a8c3f18938e4f8db86b25368e529eef
출처 데이터셋
uspto-grants-1983_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04379154

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