Butyn-2-one → 2-(3-Oxobuten-1-yl)thio-5-chloropyrimidine

HRID 905213

반응식

HRID 905213 반응식
[CH3:1][C:2](=[O:5])[C:3]#[CH:4].[Cl:6][C:7]1[CH:8]=[N:9][C:10](=[S:13])[NH:11][CH:12]=1>C(Cl)(Cl)Cl>[O:5]=[C:2]([CH3:1])[CH:3]=[CH:4][S:13][C:10]1[N:11]=[CH:12][C:7]([Cl:6])=[CH:8][N:9]=1

참가 물질

4

반응물 2

HCID 15018Butyn-2-oneHCID 71403455-Chloro-2(1H)-pyrimidinethione

생성물 1

HCID 543879192-(3-Oxobuten-1-yl)thio-5-chloropyrimidine수율 72%

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

3-Butyn-2-one (5 mmol) in chloroform (25 ml) was added dropwise over 10 min at room temperature to a stirred suspension of 5-chloropyrimidine-2-thione (4.5 mmol) in chloroform (25 ml). The mixture was stirred for an additional 10 min before the solvent was evaporated. The residue was crystallized from methanol; yield 72%, m.p. 89° C. 1H NMR (CDCl3): δ2.20 (Me-(Z)), 2.23 (Me-(E)), 6.52 (Hα, d, J 18 Hz (E)), 6.58 (Hα, d, J 10 Hz (Z)), 8.43 (Hβ, d, J 10 Hz (Z)), 8.57 (Hβ, d, J 18 Hz (E)), 8.62 (H-4, H-6); (E)/(Z)=1:1. IR (KBr): 1660 cm-1 (CO).

후처리

  1. customwas evaporated
  2. customThe residue was crystallized from methanol

출처 및 근거

ORD 기록
ord-03c3b5bc5501418ca2f992ed03b2f63b
출처 데이터셋
uspto-grants-1983_12
특허 번호
US04423047

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