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Diethyl Ether → HCID 178508793、化合物

HRID 2281574
ノート
印刷プレビュー

反応式

HRID 2281574 の反応式
[NH2:1][CH2:2][CH2:3][CH2:4][C@H:5]1[CH2:9][NH:8]/[C:7](=[N:10]\[C:11]([C:13]2[C:18]([NH2:19])=[N:17][C:16]([NH2:20])=[C:15]([Cl:21])[N:14]=2)=[O:12])/[NH:6]1.[C:22]([N:29]1[CH:33]=[CH:32]N=C1)(N1C=CN=C1)=[O:23].C(N)[C:35]1[CH:40]=[CH:39]C=[CH:37][CH:36]=1.C(OCC)C>CN(C=O)C.CO>[CH2:33]([NH:29][C:22](=[O:23])[NH:1][CH2:2][CH2:3][CH2:4][C@H:5]1[CH2:9][NH:8]/[C:7](=[N:10]\[C:11]([C:13]2[C:18]([NH2:19])=[N:17][C:16]([NH2:20])=[C:15]([Cl:21])[N:14]=2)=[O:12])/[NH:6]1)[C:32]1[CH:39]=[CH:40][CH:35]=[CH:36][CH:37]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 3283Diethyl EtherHCID 7504Benzylamine2 回HCID 682631,1'-CarbonyldiimidazoleHCID 178511031HCID 178511031、化合物

生成物 1

HCID 178508793HCID 178508793、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒
HCID 6228
Dimethylformamide
溶媒

実験手順

To a solution of 3,5-Diamino-6-chloro-pyrazine-2-carboxylic acid [(S)-4-(3-amino-propyl)-imidazolidin-(2E)-ylidene]-amide (Ex. 31) (0.040 g, 0.128 mmol) in DMF (2 ml) is added 1,1′-carbonyldiimidazole (0.023 g, 0.141 mmol) and the reaction mixture is stirred for 1 hour at room temperature. Benzylamine (0.014 ml, 0.128 mmol) is added and additional benzylamine (0.014 ml, 0.128 mmol) is added at hourly intervals for a total of 3 hours. Purification is by diluting the reaction with 2N NaOH (30 ml) and extracting the product into EtOAc (40 ml). The organic phase is washed with 2N NaOH (30 ml), dried over MgSO4 and the solvent evaporated in vacuo to yield a yellow oil. The oil is dissolved in methanol (0.75 ml) and diethyl ether (5 ml) added to triturate a yellow solid. This solid is filtered off and the filtrate formed a further precipitate. This yellow solid is collected by filtration and rinsed with diethyl ether to give the title compound; [M+H]+ 446.1

後処理

  1. customPurification
  2. additionby diluting
  3. customthe reaction with 2N NaOH (30 ml)
  4. extractionextracting the product into EtOAc (40 ml)
  5. washThe organic phase is washed with 2N NaOH (30 ml)
  6. dry with materialdried over MgSO4
  7. customthe solvent evaporated in vacuo
  8. customto yield a yellow oil
  9. customto triturate a yellow solid
  10. filtrationThis solid is filtered off
  11. customthe filtrate formed a further precipitate
  12. filtrationThis yellow solid is collected by filtration
  13. washrinsed with diethyl ether

出典と根拠

ORDレコード
ord-e9677e603658439f9fa2cb0e64b322b5
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09139586B2

反応ノート

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