p-Toluenesulfonic acid → 2-(2,3-Dihydrobenzofuran-5-yl)-1-morpholinoethanethione

HRID 868619ノート

反応式

HRID 868619 の反応式
[NH:1]1[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.[C:7]([C:10]1[CH:11]=[CH:12][C:13]2[O:17][CH2:16][CH2:15][C:14]=2[CH:18]=1)(=O)[CH3:8].[S].C1(C)C=CC([S:26](O)(=O)=O)=CC=1>CO>[O:17]1[C:13]2[CH:12]=[CH:11][C:10]([CH2:7][C:8]([N:1]3[CH2:6][CH2:5][O:4][CH2:3][CH2:2]3)=[S:26])=[CH:18][C:14]=2[CH2:15][CH2:16]1

参加物

6

反応物 4

HCID 6101p-Toluenesulfonic acidHCID 8083MorpholineHCID 1452201-(2,3-Dihydro-5-benzofuranyl)ethanoneHCID 5362487Sulfur

生成物 1

HCID 137043802-(2,3-Dihydrobenzofuran-5-yl)-1-morpholinoethanethione

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Morpholine (1.5 ml), 2,3-dihydro-5-acetylbenzofuran (2.0 g), sulfur (0.395 g) and p-toluene sulfonic acid (0.060 g) were heated at reflux. After 3 hours, the reaction mixture was cooled and 6 ml of methanol added. This solution was further cooled which precipitated the morpholide. The precipitate was filtered and washed with cold methanol to give 2,3-dihydrobenzofuran-5-ylthioacetic acid morpholide, m.p.--144°-147° C.

後処理

  1. temperatureat reflux
  2. temperaturethe reaction mixture was cooled
  3. temperatureThis solution was further cooled which
  4. customprecipitated the morpholide
  5. filtrationThe precipitate was filtered
  6. washwashed with cold methanol

出典と根拠

ORDレコード
ord-9d3301cc607748479d10fed339056f31
出典データセット
uspto-grants-1988_10
特許番号
US04780480

反応ノート

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