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Sodium → 7-benzyl-4-phenyl-6,7,8,9-tetrahydro-5H-pyrimido[4,5-d]azepine

HRID 400437
ノート
印刷プレビュー

反応式

HRID 400437 の反応式
[Na].Cl.[CH:3]([NH2:5])=[NH:4].[CH2:6]([N:13]1[CH2:19][CH2:18][C:17](Cl)=[C:16]([C:21]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)=O)[CH2:15][CH2:14]1)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1>C(O)C>[CH2:6]([N:13]1[CH2:14][CH2:15][C:16]2[C:21]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)=[N:4][CH:3]=[N:5][C:17]=2[CH2:18][CH2:19]1)[C:7]1[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 5360545SodiumHCID 10313058Methanimidamide, hydrochloride (1:1)HCID 69190815(1-benzyl-5-chloro-2,3,6,7-tetrahydro-1H-azepin-4-yl)-phenyl-methanone

生成物 1

HCID 866860407-benzyl-4-phenyl-6,7,8,9-tetrahydro-5H-pyrimido[4,5-d]azepine収率 39.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
6 °C

実験手順

16.8 g sodium was added to 500 mL ethanol at 10° C. Then, 48.5 g formamidine hydrochloride was added and the reaction was stirred 15 min at 6° C. 28 g (1-benzyl-5-chloro-2,3,6,7-tetrahydro-1H-azepin-4-yl)-phenyl-methanone was added and the reaction was stirred 17.5 h at RT and 1 h at 40° C. The mixture was filtered and the solvent was removed. The residue was dissolved in ethyl acetate. The layers were separated and the organic layer was washed with water and evaporated. The residue was crystalysed with diethylether to yield 10.7 g of the desired product. Fp: 81-82° C.

後処理

  1. stirringthe reaction was stirred 17.5 h at RT and 1 h at 40° C
  2. filtrationThe mixture was filtered
  3. customthe solvent was removed
  4. dissolutionThe residue was dissolved in ethyl acetate
  5. customThe layers were separated
  6. washthe organic layer was washed with water
  7. customevaporated

出典と根拠

ORDレコード
ord-d8ddfc66d069496abd550205319993e9
出典データセット
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08741892B2

反応ノート

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