Potassium Hydroxide → HCID 20313838, 화합물

HRID 2419129노트

반응식

HRID 2419129 반응식
[S:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[S:3][C:2]1=[N:10][CH2:11][C:12]([O:14]CC)=[O:13].[OH-].[K+]>CO>[S:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[S:3][C:2]1=[N:10][CH2:11][C:12]([OH:14])=[O:13]

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 12494980HCID 12494980, 화합물

생성물 1

HCID 20313838HCID 20313838, 화합물수율 58.5%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of [(1,3-benzodithiol-2-ylidene)amino]acetic acid ethyl ester (2.5g, prepared as described in Example 1) and potassium hydroxide (550 mg) in 500 ml of anhydrous methyl alcohol is stirred at room temperature for 120 hours. The reaction mixture is then concentrated in vacuo. The resultant solid residue is triturated with diethyl ether to remove unreacted starting material. The undissolved residue is then dissolved in 50 ml of water and filtered through Celite. The aqueous solution is treated with 10% hydrochloric acid until the pH is 5. The resultant precipitate is collected by filtration and dried in vacuo over phosphorous pentoxide at 60° C for about 16 hours. The dried solid is recrystallized twice from ethyl acetate to yield 1.3g of the title compound, melting point 195°-200° C.

후처리

  1. concentrationThe reaction mixture is then concentrated in vacuo
  2. customThe resultant solid residue is triturated with diethyl ether
  3. customto remove unreacted
  4. dissolutionThe undissolved residue is then dissolved in 50 ml of water
  5. filtrationfiltered through Celite
  6. additionThe aqueous solution is treated with 10% hydrochloric acid until the pH is 5
  7. filtrationThe resultant precipitate is collected by filtration
  8. dry with materialdried in vacuo over phosphorous pentoxide at 60° C for about 16 hours
  9. customThe dried solid is recrystallized twice from ethyl acetate

출처 및 근거

ORD 기록
ord-5e2f8028bd4b4a35b65c0ee01435c695
출처 데이터셋
uspto-grants-1978_08
특허 번호
US04104467

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