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

HRID 1701891
ノート
印刷プレビュー

反応式

HRID 1701891 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒3 回

反応条件

温度
20 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0a8c3f18938e4f8db86b25368e529eef
出典データセット
uspto-grants-1983_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04379154

反応ノート

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