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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Diethyl Ether → HCID 178508793, 화합물

HRID 1665113
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HRID 1665113 반응식
[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
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참가 물질

7

반응물 4

HCID 3283Diethyl EtherHCID 7504Benzylamine2회HCID 682631,1'-CarbonyldiimidazoleHCID 178511031HCID 178511031, 화합물

생성물 1

HCID 178508793HCID 178508793, 화합물

시약·촉매·용매 2

HCID 887Methanol용매
HCID 6228
Dimethylformamide
용매

실험 절차

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

후처리

  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

출처 및 근거

ORD 기록
ord-d20d0e9687824815b05b4057299855c0
출처 데이터셋
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08039472B2

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