Potassium Carbonate → 2-{[(6-Chloro(3-pyridyl))methyl][2-(2-ethylthio-3-nitropyrrolyl)ethyl]amino}ethanenitrile

HRID 549225ノート

反応式

HRID 549225 の反応式
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8]C(NCCCl)C#N)=[CH:4][CH:3]=1.[CH2:16]([S:18][C:19]1[NH:20][CH:21]=[CH:22][C:23]=1[N+:24]([O-:26])=[O:25])[CH3:17].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][N:20]([CH2:21][CH2:22][C:22]2[C:23]([N+:24]([O-:26])=[O:25])=[C:19]([S:18][CH2:16][CH3:17])[NH:20][CH:21]=2)[CH2:19][C:23]#[N:24])=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 598468692-Ethylthio-3-nitropyrroleHCID 86624866(6-Chloro(3-pyridyl)methyl] (2-chloroethylamino}ethanenitrile

生成物 1

HCID 866248682-{[(6-Chloro(3-pyridyl))methyl][2-(2-ethylthio-3-nitropyrrolyl)ethyl]amino}ethanenitrile

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

This compound was prepared in a manner analogous to that set forth in Step G of Example 1, using 0.17 gram (0.0007 mole) of 2-{[(6-chloro(3-pyridyl)methyl] (2-chloroethylamino}ethanenitrile (prepared in Steps A and B of the present Example), 0.10 gram (0.00064 mole) of 2-ethylthio-3-nitropyrrole and 0.22 gram (0.0016 mole) of potassium carbonate in about 15 mL of DMF. The crude product was purified with column chromatography on silica gel. Elution was accomplished using 50% hexane in diethyl ether and 100% diethyl ether as eluants. The appropriate fractions were combined and concentrated under reduced pressure, yielding 0.10 gram of Compound I. The NMR spectrum was consistent with the proposed structure.

後処理

  1. customThis compound was prepared in a manner analogous to that set forth in Step G of Example 1
  2. customThe crude product was purified with column chromatography on silica gel
  3. washElution
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-ca0ddb384ff64c89a57728bcc045cb4e
出典データセット
uspto-grants-2011_05
特許番号
US07943642B2

反応ノート

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