2-(Iodomethyl)oxirane → HCID 20475702, 화합물

HRID 905223노트

반응식

HRID 905223 반응식
[Cl:1][C:2]1[CH:3]=[N:4][C:5](=[S:8])[NH:6][CH:7]=1.[CH3:9][C:10](C)([O-:12])[CH3:11].[K+].C(C1OC1)I>CN(C=O)C>[O:12]1[CH2:11][CH:10]1[CH2:9][S:8][C:5]1[N:6]=[CH:7][C:2]([Cl:1])=[CH:3][N:4]=1

참가 물질

5

반응물 3

HCID 1646982-(Iodomethyl)oxiraneHCID 71403455-Chloro-2(1H)-pyrimidinethioneHCID 23665647Potassium tert-butoxide2회

생성물 1

HCID 20475702HCID 20475702, 화합물수율 29%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 5-chloropyrimidine-2-thione (6.9 mmol) and potassium tert-butoxide (6.9 mmol) was stirred together in anhydrous DMF (40 ml) for 5 min before epiiodohydrin (6.9 mmol) was added. The mixture was stirred at 80° C. for 7 h while small portions of potassium tert-butoxide were added from time to time to maintain a strong basic solution. The solvent was then removed at reduced pressure, the residue triturated with water (50 ml), the insoluble material extracted with chloroform and the dried (MgSO4) chloroform solution evaporated leaving the oily sulfide, yield 29%. This material was chromatographically homogenous and was identified by its spectroscopic properties. 1H NMR (CDCl3): δ2.6-3.4 (5H, m), 8.50 (H-4, H-6).

후처리

  1. additionwas added
  2. additionwere added from time to time
  3. temperatureto maintain a strong basic solution
  4. customThe solvent was then removed at reduced pressure
  5. customthe residue triturated with water (50 ml)
  6. extractionthe insoluble material extracted with chloroform
  7. dry with materialthe dried (MgSO4) chloroform solution
  8. customevaporated

출처 및 근거

ORD 기록
ord-0c0fc8113e8944a5a11f1ae0cbbb78c7
출처 데이터셋
uspto-grants-1983_12
특허 번호
US04423047

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