2-bromo-N-ethylacetamide → HCID 135828226、化合物

HRID 1784904ノート

反応式

HRID 1784904 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.[CH2:20]([NH:22][C:23](=[O:26])[CH2:24]Br)[CH3:21].C([O-])(O)=O.[Na+]>CN(C=O)C>[NH2:1][C:2]1[N:3]=[C:4]([S:19][CH2:24][C:23]([NH:22][CH2:20][CH3:21])=[O:26])[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

5

反応物 3

HCID 2207922-bromo-N-ethylacetamideHCID 516892Sodium BicarbonateHCID 178510481HCID 178510481、化合物

生成物 1

HCID 135828226HCID 135828226、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

At RT 0.76 g (2 mmol) of 2-amino-4-(4-hydroxyphenyl)-6-sulfanyl-3,5-pyridinedicarbonitrile and 0.5 g (3 mmol) of N-ethylbromoacetamide are stirred in 5 ml of DMF together with 0.34 g (4 mmol) of NaHCO3 for 4 hours. After dilution with water, the mixture is extracted with ethyl acetate and the ethyl acetate phase is dried with MgSO4 and concentrated under reduced pressure. The solid residue obtained after concentration is stirred with methanol. The crystals are filtered off with suction and dried under reduced pressure.

後処理

  1. extractionAfter dilution with water, the mixture is extracted with ethyl acetate
  2. dry with materialthe ethyl acetate phase is dried with MgSO4
  3. concentrationconcentrated under reduced pressure
  4. customThe solid residue obtained
  5. concentrationafter concentration
  6. filtrationThe crystals are filtered off with suction
  7. customdried under reduced pressure

出典と根拠

ORDレコード
ord-78fedb32620646d5b1f94b66e481d520
出典データセット
uspto-grants-2009_03
特許番号
US07504421B2

反応ノート

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