Methyl isothiocyanate → HCID 10198239、化合物
反応式
[C:1]([C:5]1[CH2:6][CH2:7][NH:8][CH2:9][CH:10]=1)([CH3:4])([CH3:3])[CH3:2].[CH3:11][N:12]=[C:13]=[S:14]>O1CCCC1>[CH3:11][NH:12][C:13]([N:8]1[CH2:7][CH:6]=[C:5]([C:1]([CH3:4])([CH3:3])[CH3:2])[CH2:10][CH2:9]1)=[S:14]参加物
4
実験手順
In 60 ml. of ml.of anhydrous tetrahydrofuran, there is dissolved 12.0 grams of 4-t-butyl-1,2,3,6-tetrahydropyridine. Stirring is initiated and there is added 7.3 grams of methylisothiocyanate in 25 ml. of anhydrous tetrahydrofuran. After stirring the reaction mixture for 18 hours at room temperature, the tetrahydrofuran is evaporated in vacuo at 50°C/20 mmHg. The resulting oil is crystallized from methylene chloride/pentane 1:1 to give N-methyl-4-t-butyl-1,2,3,6-tetrahydro-1-pyridinethiocarboxamide; m.p. 76° to 78°C.
後処理
- stirringAfter stirring the reaction mixture for 18 hours at room temperature
- customthe tetrahydrofuran is evaporated in vacuo at 50°C/20 mmHg
- customThe resulting oil is crystallized from methylene chloride/pentane 1:1
出典と根拠
- ORDレコード
- ord-1117535de9714f158046d36e0d73596c
- 出典データセット
- uspto-grants-1976_08
- 特許番号
- US03974283
反応ノート
読み込み中…