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Hydrogen Sulfide → 2-(Morpholin-4-yl)ethanethioamide

HRID 358478
ノート
印刷プレビュー

反応式

HRID 358478 の反応式
C(N(CC)CC)C.[O:8]1[CH2:13][CH2:12][N:11]([CH2:14][C:15]#[N:16])[CH2:10][CH2:9]1.[SH2:17]>N1C=CC=CC=1>[O:8]1[CH2:13][CH2:12][N:11]([CH2:14][C:15]([NH2:16])=[S:17])[CH2:10][CH2:9]1
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 402Hydrogen SulfideHCID 8471TriethylamineHCID 220554-Morpholineacetonitrile

生成物 1

HCID 38476342-(Morpholin-4-yl)ethanethioamide

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A reaction mixture was prepared from 203 ml. each of triethylamine and pyridine plus 63 g. of morpholinoacetonitrile. Hydrogen sulfide was bubbled through the heated, stirred reaction mixture for about 2.5 hours. Stirring was continued overnight at ambient temperature. The next day, H2S was passed through the heated, stirred reaction mixture for an additional 1.5 hours. At this point, the solvents were evaporated in vacuo and the residue triturated with ether. The ether was discarded and the residue dissolved in ethanol. Crystalline morpholinothioacetamide formed in the above reaction precipitated and was separated by filtration. Treatment of the filtrate with alcoholic hydrogen chloride yielded morpholinothioacetamide hydrochloride melting in the range 64°-80° C. See also J.A.C.S., 72, 2804 (1950).

後処理

  1. customA reaction mixture was prepared from 203 ml
  2. customHydrogen sulfide was bubbled through the heated
  3. customreaction mixture for about 2.5 hours
  4. stirringStirring
  5. stirringstirred
  6. customreaction mixture for an additional 1.5 hours
  7. customAt this point, the solvents were evaporated in vacuo
  8. customthe residue triturated with ether
  9. dissolutionthe residue dissolved in ethanol

出典と根拠

ORDレコード
ord-a7bb75664c5245558b09f8612ee5d2ae
出典データセット
uspto-grants-1984_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04468399

反応ノート

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