3-[[5-[4-(1,1-Dimethylethyl)phenyl]-1,2,3-thiadiazol-4-yl]thio]propanoic acid, ethyl ester → HCID 14294241, 화합물

HRID 1381712노트

반응식

HRID 1381712 반응식
[CH3:1][C:2]([C:5]1[CH:10]=[CH:9][C:8]([C:11]2[S:15][N:14]=[N:13][C:12]=2[S:16]CCC(OCC)=O)=[CH:7][CH:6]=1)([CH3:4])[CH3:3].[O-]CC.[K+]>C(O)C>[CH3:4][C:2]([C:5]1[CH:6]=[CH:7][C:8]([C:11]2[S:15][N:14]=[N:13][C:12]=2[SH:16])=[CH:9][CH:10]=1)([CH3:1])[CH3:3]

참가 물질

4

반응물 2

HCID 142942003-[[5-[4-(1,1-Dimethylethyl)phenyl]-1,2,3-thiadiazol-4-yl]thio]propanoic acid, ethyl esterHCID 23670592Potassium ethoxide

생성물 1

HCID 14294241HCID 14294241, 화합물수율 114.5%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

A solution of 15.9 g of 3-[[5-[4-(1,1-dimethylethyl)phenyl]-1,2,3-thiadiazol-4-yl]thio]propanoic acid, ethyl ester in 75 ml of anhydrous ethanol was treated with 105 ml of 0.5M potassium ethoxide in ethanol. After 3 hours the solvent was partially removed in vacuo and 200 ml of anhydrous ether was added. The resulting solid was collected, washed with ether, redissolved in methanol, filtered and the filtrate concentrated to 10-15 ml. A 250 ml portion of anhydrous ether was added and the solid was collected and dried in vacuo, giving 13 g of 5-[4-(1,1-dimethylethyl)phenyl]-1,2,3-thiadiazol-4-thiol, potassium salt as a yellow solid, mp >150° C.

후처리

  1. customAfter 3 hours the solvent was partially removed in vacuo and 200 ml of anhydrous ether
  2. additionwas added
  3. customThe resulting solid was collected
  4. washwashed with ether
  5. dissolutionredissolved in methanol
  6. filtrationfiltered
  7. concentrationthe filtrate concentrated to 10-15 ml
  8. additionA 250 ml portion of anhydrous ether was added
  9. customthe solid was collected
  10. customdried in vacuo

출처 및 근거

ORD 기록
ord-a3eaf5db50344522bd88863aa2ba9ffb
출처 데이터셋
uspto-grants-1989_02
특허 번호
US04803280

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