Sodium ethoxide → (7-benzyl-6,7,8,9-tetrahydro-5H-pyrimido[4,5-d]azepin-2-yl)-phenyl-amine

HRID 400465노트

반응식

HRID 400465 반응식
Cl.[CH2:2]([N:9]1[CH2:15][CH2:14][C:13](Cl)=[C:12]([CH:17]=O)[CH2:11][CH2:10]1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[CH:19]1[CH:24]=[CH:23][C:22]([N:25]=[C:26]([NH2:28])[NH2:27])=[CH:21][CH:20]=1.C(O)(O)=O.C([O-])C.[Na+]>C(O)C>[CH2:2]([N:9]1[CH2:10][CH2:11][C:12]2[CH:17]=[N:27][C:26]([NH:25][C:22]3[CH:23]=[CH:24][CH:19]=[CH:20][CH:21]=3)=[N:28][C:13]=2[CH2:14][CH2:15]1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1

참가 물질

5

반응물 3

HCID 2723922Sodium ethoxideHCID 16217093Carbonic acid, compound with phenylguanidine (1:1)HCID 189435411-benzyl-5-chloro-2,3,6,7-tetrahydro-1H-azepine-4-carbaldehyde hydrochloride

생성물 1

HCID 86686075(7-benzyl-6,7,8,9-tetrahydro-5H-pyrimido[4,5-d]azepin-2-yl)-phenyl-amine수율 26%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
70 °C

실험 절차

1 g 1-benzyl-5-chloro-2,3,6,7-tetrahydro-1H-azepine-4-carbaldehyde hydrochloride was added to 1 g phenylguanidine carbonate salt and 1 g sodium ethanolate in 25 mL ethanol. The reaction was stirred 4 h at 70° C. The mixture was filtered over silica gel and the solvent was removed. The residue was purified by chromatography on silica gel (dichlormethane/MeOH/ammonia: 19/1/0.1) to yield 300 mg of the desired product.

후처리

  1. filtrationThe mixture was filtered over silica gel
  2. customthe solvent was removed
  3. customThe residue was purified by chromatography on silica gel (dichlormethane/MeOH/ammonia: 19/1/0.1)

출처 및 근거

ORD 기록
ord-afee4ea0a0fa4078a729b243170162ac
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08741892B2

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