p-Toluenesulfonic acid monohydrate → 5,6,7,7a-Tetrahydrothieno[3,2-c]pyridin-2(4H)-one

HRID 363719노트

반응식

HRID 363719 반응식
C([N:20]1[CH2:25][CH2:24][CH:23]2[S:26][C:27](=[O:29])[CH:28]=[C:22]2[CH2:21]1)(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>O1CCCC1>[S:26]1[CH:23]2[C:22]([CH2:21][NH:20][CH2:25][CH2:24]2)=[CH:28][C:27]1=[O:29]

참가 물질

4

반응물 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 137484625-(Triphenylmethyl)-5,6,7,7a-tetrahydrothieno[3,2-c]pyridin-2(4H)-one

생성물 1

HCID 137484635,6,7,7a-Tetrahydrothieno[3,2-c]pyridin-2(4H)-one수율 204.9%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
50 °C

실험 절차

A mixture of 2.85 g of 5-trityl-5,6,7,7a-tetrahydro-4H-thieno [3,2-c]pyridin-2-one (see Japanese Provisional Patent Publication No. 246148/1986), 1.36 g of p-toluenesulfonic acid monohydrate and 50 ml of tetrahydrofuran was stirred at 50° C. for 2 hours. The precipitated solid was filtered, washed with 10 ml of tetrahydrofuran and then dried to obtain 2.28 g of 5,6,7,7a-tetrahydro-4H-thieno[3,2-c]-pyridin-2one.p-toluenesulfonate (yield based on 5-trityl-5,6,7,7a-tetrahydro-4H-thieno[3,2-c]pyridin-2-one: 93%).

후처리

  1. filtrationThe precipitated solid was filtered
  2. washwashed with 10 ml of tetrahydrofuran
  3. customdried

출처 및 근거

ORD 기록
ord-b929c7c39bad42fcaa6dc30e33ddafab
출처 데이터셋
uspto-grants-1999_02
특허 번호
US05874581

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