Sodium Bicarbonate → HCID 135828236、化合物

HRID 720449ノート

反応式

HRID 720449 の反応式
[NH2:1][C:2]1[C:7]([C:8]#[N:9])=[C:6]([C:10]2[CH:15]=[CH:14][C:13]([OH:16])=[CH:12][CH:11]=2)[C:5]([C:17]#[N:18])=[C:4]([SH:19])[N:3]=1.[CH3:20][NH:21][C:22](=[O:25])[CH2:23]Br.C([O-])(O)=O.[Na+].C(Cl)Cl.CO>CN(C)C=O.O.C(OCC)(=O)C>[NH2:1][C:2]1[N:3]=[C:4]([S:19][CH2:23][C:22]([NH:21][CH3:20])=[O:25])[C:5]([C:17]#[N:18])=[C:6]([C:10]2[CH:11]=[CH:12][C:13]([OH:16])=[CH:14][CH:15]=2)[C:7]=1[C:8]#[N:9]

参加物

8

反応物 4

HCID 516892Sodium BicarbonateHCID 154907452-Bromo-N-methylacetamideHCID 21226129Dichloromethane methanolHCID 178510481HCID 178510481、化合物

生成物 1

HCID 135828236HCID 135828236、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

At room temperature (RT), 53.6 mg (0.2 mmol) of 2-amino-4-(4-hydroxyphenyl)-6-sulfanyl-3,5-pyridinedicarbonitrile and 45.6 mg (0.3 mmol) of N-methylbromoacetamide are stirred in 0.5 ml of dimethylformamide (DMF) together with 33.6 mg (0.4 mmol) of NaHCO3 for 4 hours. Thin-layer chromatography (TLC) (CH2Cl2/CH3OH 10:1) shows complete conversion. The entire mixture is diluted with water and ethyl acetate (EA) and the EA phase is dried with MgSO4 and concentrated under reduced pressure. The residue crystallizes from methanol.

後処理

  1. dry with materialthe EA phase is dried with MgSO4
  2. concentrationconcentrated under reduced pressure
  3. customThe residue crystallizes from methanol

出典と根拠

ORDレコード
ord-0cedceb4c08f46e5bdf40a55b4b3159f
出典データセット
uspto-grants-2006_11
特許番号
US07135486B1

反応ノート

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