Iodoacetamide → HCID 20475727、化合物

反応式

Cl.[CH3:2][C:3]1[C:8]([Br:9])=[C:7]([CH3:10])[NH:6][C:5](=[S:11])[N:4]=1.[OH-].[K+].I[CH2:15][C:16]([NH2:18])=[O:17]>>[C:16]([CH2:15][S:11][C:5]1[N:6]=[C:7]([CH3:10])[C:8]([Br:9])=[C:3]([CH3:2])[N:4]=1)(=[O:17])[NH2:18]

参加物

反応物 3

HCID 3727Iodoacetamide

HCID 14797Potassium Hydroxide

HCID 20475758HCID 20475758、化合物

生成物 1

HCID 20475727HCID 20475727、化合物収率 72%

実験手順

4,6-Dimethyl-5-bromopyrimidine-2-thione HCl salt (5 mmol) was added to ethanolic (60 ml) KOH (11.4 mmol), the solution stirred for 10 min at room temperature, iodoacetamide (5.7 mmol) added, the stirring continued for 20 min at room temperature and for 100 min at 70° C. (pH 8). The warm reaction mixture was filtered, the filtrate evaporated, the residue extracted with chloroform (150 ml), the chloroform solution washed and the dried (MgSO4) solution evaporated to leave the sulfide; yield 72%, m.p. 175°-177° C. (iPrOH). 1H NMR (DMSO-d6): δ2.50 (Me), 3.80 (SCH2).

後処理

waitthe stirring continued for 20 min at room temperature and for 100 min at 70° C.
customThe warm reaction mixture
filtrationwas filtered
customthe filtrate evaporated
extractionthe residue extracted with chloroform (150 ml)
washthe chloroform solution washed
dry with materialthe dried (MgSO4) solution
customevaporated

出典と根拠

ORDレコード: ord-f8ddfa65af6b4e8a8b3021742794d2bf
出典データセット: uspto-grants-1983_12
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US04423047

反応ノート

読み込み中…

参加物