Ethanol → 5-[3,5-bis(1,1-dimethylethyl)-4-hydroxyphenyl]-1,3,4-thiadiazole-2(3H)-thione calcium

HRID 1657081노트

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HRID 1657081 반응식
O.O.[Cl-].[Ca+2:4].[Cl-].[CH3:6][C:7]([C:10]1[CH:11]=[C:12]([C:21]2[S:25][C:24](=[S:26])[NH:23][N:22]=2)[CH:13]=[C:14]([C:17]([CH3:20])([CH3:19])[CH3:18])[C:15]=1[OH:16])([CH3:9])[CH3:8].C(O)C>O1CCCC1>[Ca:4].[CH3:9][C:7]([C:10]1[CH:11]=[C:12]([C:21]2[S:25][C:24](=[S:26])[NH:23][N:22]=2)[CH:13]=[C:14]([C:17]([CH3:18])([CH3:19])[CH3:20])[C:15]=1[OH:16])([CH3:6])[CH3:8]

참가 물질

5

반응물 3

HCID 702EthanolHCID 30370185-(3,5-Di-tert-butyl-4-hydroxyphenyl)-1,3,4-thiadiazole-2(3H)-thioneHCID 6093260Calcium chloride, dihydrate

생성물 1

HCID 1364033995-[3,5-bis(1,1-dimethylethyl)-4-hydroxyphenyl]-1,3,4-thiadiazole-2(3H)-thione calcium수율 127.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Calcium chloride dihydrate (1.496, 0.0102 mole) is added in one portion to a solution of 5-[3,5-bis(1,1-dimethylethyl)-4-hydroxy-phenyl]-1,3,4-thiadiazole-2(3H)-thione (8.11 g, 0.0204 mole) in tetrahydrofuran (80 ml). The resulting mixture is stirred hours at room temperature before absolute ethanol (80 ml) is added. The mixture is stirred overnight at room temperature. The solution is concentrated in vacuo and the residue dissolved in tetrahydrofuran and the product is precipitated by the addition of water. Filtration and drying at 80° C. in vacuo provides 4.7 g (6.8 g theor., 68%) 5-[3,5-bis(1,1-dimethylethyl)-4-hydroxyphenyl]-1,3,4-thiadiazole-2(3H)-thione calcium (2:1) (salt), mp 212°-231° C., analyzed for 0.31 hydrate.

후처리

  1. additionis added
  2. concentrationThe solution is concentrated in vacuo
  3. dissolutionthe residue dissolved in tetrahydrofuran
  4. customthe product is precipitated by the addition of water
  5. filtrationFiltration
  6. customdrying at 80° C. in vacuo

출처 및 근거

ORD 기록
ord-840ff941115a46de9dec80d26440e3bc
출처 데이터셋
uspto-grants-1993_10
특허 번호
US05256680

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