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

HRID 868619노트

반응식

HRID 868619 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9d3301cc607748479d10fed339056f31
출처 데이터셋
uspto-grants-1988_10
특허 번호
US04780480

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