N-(2,6-dichloropyrimidin-4-yl)acetamide → N-{2-Chloro-6-[1-(3-ethoxy-4-methoxy-benzyl)-piperidin-4-ylamino]-pyrimidin-4-yl}-acetamide

HRID 2426539

반응식

HRID 2426539 반응식
[Cl:1][C:2]1[N:7]=[C:6]([NH:8][C:9](=[O:11])[CH3:10])[CH:5]=[C:4](Cl)[N:3]=1.[CH2:13]([O:15][C:16]1[CH:17]=[C:18]([CH:27]=[CH:28][C:29]=1[O:30][CH3:31])[CH2:19][N:20]1[CH2:25][CH2:24][CH:23]([NH2:26])[CH2:22][CH2:21]1)[CH3:14]>CC(N(C)C)=O>[Cl:1][C:2]1[N:7]=[C:6]([NH:8][C:9](=[O:11])[CH3:10])[CH:5]=[C:4]([NH:26][CH:23]2[CH2:24][CH2:25][N:20]([CH2:19][C:18]3[CH:27]=[CH:28][C:29]([O:30][CH3:31])=[C:16]([O:15][CH2:13][CH3:14])[CH:17]=3)[CH2:21][CH2:22]2)[N:3]=1

참가 물질

4

반응물 2

HCID 4713752N-(2,6-dichloropyrimidin-4-yl)acetamideHCID 392574451-(3-Ethoxy-4-methoxy-benzyl)-piperidin-4-ylamine2회

생성물 1

HCID 86618534N-{2-Chloro-6-[1-(3-ethoxy-4-methoxy-benzyl)-piperidin-4-ylamino]-pyrimidin-4-yl}-acetamide수율 3%

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

실험 절차

A solution of N-(2,6-dichloro-pyrimidin-4-yl)-acetamide (30.9 mg, 0.15 mmol, 1.0 equiv) and 1-(3-ethoxy-4-methoxy-benzyl)-piperidin-4-ylamine (47.6 mg, 0.18 mmol, 1.2 equiv; intermediate A1) in DMAc (2 mL) was heated by microwave irradiation to 180° C. for 15 min. Removal of the solvent under reduced pressure and purification by preparative HPLC on reversed phase eluting with a gradient of acetonitrile/water provided 1.6 mg (3%) of the title compound. MS (ISP): 434.4 [M+H]+.

후처리

  1. customRemoval of the solvent
  2. customunder reduced pressure and purification by preparative HPLC on reversed phase
  3. washeluting with a gradient of acetonitrile/water

출처 및 근거

ORD 기록
ord-7a741dd6a00a4ce3bcc0392de29e799b
출처 데이터셋
uspto-grants-2011_06
특허 번호
US07968568B2

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