Water → HCID 86685596, 화합물

HRID 2200479노트

반응식

HRID 2200479 반응식
[Cl:1][C:2]1[C:3]([C:9]#[N:10])=[N:4][CH:5]=[C:6](Cl)[N:7]=1.Cl.[NH2:12][C:13]1([C:17]([NH2:19])=[O:18])[CH2:16][CH2:15][CH2:14]1.CCN(C(C)C)C(C)C.O>CN(C=O)C.CCOC(C)=O>[Cl:1][C:2]1[N:7]=[C:6]([NH:12][C:13]2([C:17]([NH2:19])=[O:18])[CH2:16][CH2:15][CH2:14]2)[CH:5]=[N:4][C:3]=1[C:9]#[N:10]

참가 물질

7

반응물 4

HCID 962WaterHCID 81531DiisopropylethylamineHCID 529877443,5-Dichloropyrazine-2-carbonitrileHCID 717569071-Aminocyclobutane-1-carboxamide hydrochloride

생성물 1

HCID 86685596HCID 86685596, 화합물수율 15.2%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

A solution of 3,5-dichloropyrazine-2-carbonitrile (100 mg, 0.574 mmol), 1-aminocyclobutanecarboxamide hydrochloride (108 mg, 0.717 mmol) and DIEA (0.350 mL, 2.01 mmol) in DMF (4 mL) was stirred at room temperature for 70 h. Water and EtOAc were added. Organic phase was separated, washed with 1N HCl, then with 5% NaHCO3, dried over Na2SO4, concentrated in vacuo. The residue was purified by HPLC to give 1-(6-chloro-5-cyanopyrazin-2-ylamino)cyclobutanecarboxamide (22 mg).

후처리

  1. customOrganic phase was separated
  2. washwashed with 1N HCl
  3. dry with materialwith 5% NaHCO3, dried over Na2SO4
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by HPLC

출처 및 근거

ORD 기록
ord-9b932c5a0c204f47bdaa5045a8c95119
출처 데이터셋
uspto-grants-2016_06
특허 번호
US09359308B2

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