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Methyl isothiocyanate → (+/-)-N-methyl-2-oxo-1-(3-quinolinyl)cyclohexanecarbothioamide

HRID 5909
ノート
印刷プレビュー

反応式

HRID 5909 の反応式
[N:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[C:3]([CH:11]2[CH2:16][CH2:15][CH2:14][CH2:13][C:12]2=[O:17])[CH:2]=1.CC(C)([O-])C.[K+].[CH3:24][N:25]=[C:26]=[S:27]>O1CCCC1>[CH3:24][NH:25][C:26]([C:11]1([C:3]2[CH:2]=[N:1][C:10]3[C:5]([CH:4]=2)=[CH:6][CH:7]=[CH:8][CH:9]=3)[CH2:16][CH2:15][CH2:14][CH2:13][C:12]1=[O:17])=[S:27]
参加物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 11167Methyl isothiocyanateHCID 19794569(+/-)-2-(3-Quinolinyl)cyclohexanoneHCID 23665647Potassium tert-butoxide

生成物 1

HCID 19794596(+/-)-N-methyl-2-oxo-1-(3-quinolinyl)cyclohexanecarbothioamide収率 9.4%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of (±)-2-(quinolin-3-yl)cyclohexanone (0.78 g, 3.5 mmol) in tetrahydrofuran (10 ml) at -5° C. was treated with potassium t-butoxide (0.43 g, 3.9 mmol) in one portion. After 25 minutes at -5° C. the deep red mixture was treated dropwise during 1 minute with a solution of methyl isothiocyanate (0.28 g, 3.9 mmol) in tetrahydrofuran (2 ml). After 4 hours at 0° C. the reaction mixture was partitioned between saturated aqueous ammonium chloride solution (50 ml) and chloroform (50 ml). The aqueous layer was extracted again with chloroform (50 ml). The combined organic extracts were then dried over sodium sulphate and concentrated in vacuo (20° C.; 14 mmHg) to give a crude oil which was purified by flash chromatography over silica gel eluting with ethyl acetate to give (±)-N-methyl-2-oxo-1-(quinolin-3-yl)cyclohexanecarbothioamide (0.1 g, 0.33 mmol), m.p. 235°-236° C.;

後処理

  1. customAfter 4 hours at 0° C. the reaction mixture was partitioned between saturated aqueous ammonium chloride solution (50 ml) and chloroform (50 ml)
  2. extractionThe aqueous layer was extracted again with chloroform (50 ml)
  3. dry with materialThe combined organic extracts were then dried over sodium sulphate
  4. concentrationconcentrated in vacuo (20° C.; 14 mmHg)
  5. customto give a crude oil which
  6. customwas purified by flash chromatography over silica gel eluting with ethyl acetate

出典と根拠

ORDレコード
ord-437552d324044abea55731a4552ead93
出典データセット
uspto-grants-1993_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05246950

反応ノート

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