Imidazo[2,1-b]thiazole-6-methanol, 2,3-dihydro-, 1,1-dioxide → HCID 18183096, 화합물

HRID 1450681노트

반응식

HRID 1450681 반응식
[OH:1][CH2:2][C:3]1[N:4]=[C:5]2[N:9]([CH:10]=1)[CH2:8][CH2:7][S:6]2(=[O:12])=[O:11]>C(#N)C.[O-2].[O-2].[Mn+4]>[S:6]1(=[O:12])(=[O:11])[CH2:7][CH2:8][N:9]2[CH:10]=[C:3]([CH:2]=[O:1])[N:4]=[C:5]12

참가 물질

4

반응물 1

HCID 18183097Imidazo[2,1-b]thiazole-6-methanol, 2,3-dihydro-, 1,1-dioxide

생성물 1

HCID 18183096HCID 18183096, 화합물

시약·촉매·용매 2

HCID 178418406HCID 178418406, 화합물촉매2회HCID 6342Acetonitrile용매

실험 절차

2,3-Dihydro-6-hydroxymethylimidazo[2,1-b]thiazole- 1,1-dioxide (207 mg, 1.1 mmol) was dissolved in acetonitrile (minimum volume) and treated with manganese dioxide (621 mg, 3 wt. equivalents) and the mixture stirred vigorously at ambient temperature. After 1 h, more manganese dioxide (621 mg) was added and the mixture sitrred for a further 18 h. The mixture was filtered through Celite, the filter bed washed with acetonitrile, the filtrate and washings combined and evaporated to dryness under reduced pressure. The residue was triturated under dichloromethane and the resulting solid collected by filtration, washed with dichloromethane and dried in air (108 mg, 53%) (Found: M+ 186.0103. C6H6N2O3S requires M 186.0099); νmax (Nujol) 1691, 1320 and 1132 cm-1 ; δH [250 MHz; (CD3)2SO]4.25 (2H, t, J 7 Hz), 4.68 (2H, t, J7 Hz), 8.32 (1H, s), 9.81 (1H, s).

후처리

  1. waitthe mixture sitrred for a further 18 h
  2. filtrationThe mixture was filtered through Celite
  3. washthe filter bed washed with acetonitrile
  4. customevaporated to dryness under reduced pressure
  5. customThe residue was triturated under dichloromethane
  6. filtrationthe resulting solid collected by filtration
  7. washwashed with dichloromethane
  8. customdried in air (108 mg, 53%) (Found: M+ 186.0103. C6H6N2O3S requires M 186.0099)

출처 및 근거

ORD 기록
ord-289f69bbffa2458cbcbb28341b5685cd
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05602250

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