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Hydrochloric Acid → HCID 20430559, 화합물

HRID 2413127
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HRID 2413127 반응식
[O:1]=[C:2]1[CH2:7][N:6](S(C2C=CC(C)=CC=2)(=O)=O)[CH2:5][C:4]2[CH:18]=[CH:19][S:20][C:3]1=2.CC(C)([O-])C.[K+].Cl>C(O)(C)(C)C>[OH:1][C:2]1[C:3]2[S:20][CH:19]=[CH:18][C:4]=2[CH:5]=[N:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 12751998HCID 12751998, 화합물HCID 23665647Potassium tert-butoxide

생성물 1

HCID 20430559HCID 20430559, 화합물수율 72%

시약·촉매·용매 1

HCID 6386tert-Butanol용매

실험 절차

A solution of 7-oxo-5-tosyl-4,5,6,7-tetrahydro-thieno[3,2-c]pyridine (19.6 g; 0.064 mole; obtained in (b) above) and potassium tert-butoxide (28.6 g; 0.255 mole) in tert-butanol (300 ml) is refluxed for 2 hours under a nitrogen atmosphere. Evaporation of the solvent in vacuo leaves a residue which is taken up into 2N hydrochloric acid. The aqueous phase is extracted with ether, made basic by addition of concentrated ammonia, and evaporated to dryness. The residue is extracted four times with boiling ethyl acetate. The organic extracts are filtered through a silica bed and evaporated to dryness. The solid residue is recrystallized from ethanol-acetonitrile. Greyish crystals; M.P.=180° C.; Yield: 72%.

후처리

  1. customEvaporation of the solvent in vacuo
  2. customleaves a residue which
  3. extractionThe aqueous phase is extracted with ether
  4. additionmade basic by addition of concentrated ammonia
  5. customevaporated to dryness
  6. extractionThe residue is extracted four times with boiling ethyl acetate
  7. filtrationThe organic extracts are filtered through a silica bed
  8. customevaporated to dryness
  9. customThe solid residue is recrystallized from ethanol-acetonitrile

출처 및 근거

ORD 기록
ord-4e2e22798c1045feb3ba95a9bf93cf75
출처 데이터셋
uspto-grants-1985_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04496568

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