2-(Iodomethyl)oxirane → HCID 20475702、化合物

HRID 905223ノート

反応式

HRID 905223 の反応式
[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

参加物

5

反応物 3

HCID 1646982-(Iodomethyl)oxiraneHCID 71403455-Chloro-2(1H)-pyrimidinethioneHCID 23665647Potassium tert-butoxide2 回

生成物 1

HCID 20475702HCID 20475702、化合物収率 29%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-0c0fc8113e8944a5a11f1ae0cbbb78c7
出典データセット
uspto-grants-1983_12
特許番号
US04423047

反応ノート

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