Tetrahydrofuran → 4-(1,3-Dithiol-2-ylidene)morpholinium perchlorate

HRID 648909

반응식

HRID 648909 반응식
O1CCCC1.[NH:6]1[CH2:11][CH2:10][O:9][CH2:8][CH2:7]1.[Cl:12]([O-:16])(=[O:15])(=[O:14])=[O:13].CS[C:19]1[S:23][CH:22]=[CH:21][S+:20]=1>C(O)C>[Cl:12]([O-:16])(=[O:15])(=[O:14])=[O:13].[S:20]1[CH:21]=[CH:22][S:23][C:19]1=[N+:6]1[CH2:11][CH2:10][O:9][CH2:8][CH2:7]1

참가 물질

5

반응물 3

HCID 8028TetrahydrofuranHCID 8083MorpholineHCID 230390092-Methylthio-1,3-dithiolium perchlorate

생성물 1

HCID 136549514-(1,3-Dithiol-2-ylidene)morpholinium perchlorate수율 83.3%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To 20 ml of tetrahydrofuran, 1.0 ml of morpholine was dissolved, and 2.5 g of 2-methylthio-1,3-dithiolium perchlorate was gradually added thereto under stirring at room temperature. The mixture was stirred at room temperature for 1 hour, and then the precipitated crystals were collected by filtration and recrystallized from ethanol, whereby 2.4 g (yield: 83.3%) of 4-(1,3-dithiol-2-ylidene)morpholinium perchlorate (Compound No. 26) was obtained as crystals having a melting point of from 177° to 178° C.

후처리

  1. stirringThe mixture was stirred at room temperature for 1 hour
  2. filtrationthe precipitated crystals were collected by filtration

출처 및 근거

ORD 기록
ord-9325cdc0622a42d09fa36230fa4b2101
출처 데이터셋
uspto-grants-1988_04
특허 번호
US04737494

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