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Hydrochloric Acid → 2-Sulfamoyl-4,5,6,7-tetrahydrothieno[2,3-c]pyridine

HRID 569048
노트
인쇄 미리보기

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HRID 569048 반응식
[S:1]([C:5]1[S:16][C:8]2[CH2:9][N:10](C(=O)C)[CH2:11][CH2:12][C:7]=2[CH:6]=1)(=[O:4])(=[O:3])[NH2:2].Cl.C(=O)([O-])[O-].[Na+].[Na+].C(OCC)(=O)C.CO>[OH-].[Na+]>[S:1]([C:5]1[S:16][C:8]2[CH2:9][NH:10][CH2:11][CH2:12][C:7]=2[CH:6]=1)(=[O:3])(=[O:4])[NH2:2]
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참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 10340Sodium CarbonateHCID 201485722-Sulfamoyl-6-acetyl-4,5,6,7-tetrahydrothieno[2,3-c]pyridineHCID 21584119Ethylacetate methanol

생성물 1

HCID 201485892-Sulfamoyl-4,5,6,7-tetrahydrothieno[2,3-c]pyridine수율 91.1%

시약·촉매·용매 1

HCID 14798
Sodium Hydroxide
용매

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온도
80 °C

실험 절차

A suspension of 2-sulfamoyl-6-acetyl-4,5,6,7-tetrahydrothieno[2,3-c]pyridine (9.61 g, 37 mmol) in 20% sodium hydroxide solution (75 ml) was warmed at 80° C. for 3 hours. The resultant clear solution was cooled, acidified with concentrated hydrochloric acid, and then made basic with saturated sodium carbonate solution. The product was isolated by exhaustive extraction into ethyl acetate/methanol. The dried solution was evaporated to give 7.36 g (91% yield) of product. Recrystallization from ethyl acetate/methanol gave pure product; m.p. 172°-175° C.

후처리

  1. temperatureThe resultant clear solution was cooled
  2. customThe dried solution was evaporated

출처 및 근거

ORD 기록
ord-c67af48a0b7f4bc989bceca52911f178
출처 데이터셋
uspto-grants-1988_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04731368

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