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Hydrochloric Acid → HCID 20430559、化合物

HRID 2413127
ノート
印刷プレビュー

反応式

HRID 2413127 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 12751998HCID 12751998、化合物HCID 23665647Potassium tert-butoxide

生成物 1

HCID 20430559HCID 20430559、化合物収率 72%

試薬・触媒・溶媒 1

HCID 6386tert-Butanol溶媒

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-4e2e22798c1045feb3ba95a9bf93cf75
出典データセット
uspto-grants-1985_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04496568

反応ノート

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