2-bromo-N,N-diethylacetamide → HCID 135828231、化合物

HRID 720450ノート

反応式

HRID 720450 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]([N:22]([CH2:27][CH3:28])[C:23](=[O:26])[CH2:24]Br)[CH3:21].C([O-])(O)=O.[Na+].C(Cl)Cl.CO>CN(C=O)C.O.C(OCC)(=O)C>[NH2:1][C:2]1[N:3]=[C:4]([S:19][CH2:24][C:23]([N:22]([CH2:27][CH3:28])[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

8

反応物 4

HCID 2255452-bromo-N,N-diethylacetamideHCID 516892Sodium BicarbonateHCID 21226129Dichloromethane methanolHCID 178510481HCID 178510481、化合物

生成物 1

HCID 135828231HCID 135828231、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 RT, 53.6 mg (0.2 mmol) of 2-amino-4-(4-hydroxyphenyl)-6-sulfanyl-3,5-pyridinedicarbonitrile and 58.2 mg (0.3 mmol) of N,N-diethylbromoacetamide are stirred in 0.5 ml of DMF together with 33.6 mg (0.4 mmol) of NaHCO3 for 4 hours. TLC (CH2Cl2/CH3OH 10:1) shows complete conversion. The entire mixture is diluted with water and ethyl acetate 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-57c24c9c4d4b4f118c2b63c439fffa3e
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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