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

HRID 400465ノート

反応式

HRID 400465 の反応式
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

参加物

5

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
70 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-afee4ea0a0fa4078a729b243170162ac
出典データセット
uspto-grants-2014_06
特許番号
US08741892B2

反応ノート

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