ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Benzaldehyde → 3-Amino-1-benzyl-3-[4-(benzyloxy)benzyl]azepan-2-one

HRID 1271491
ノート
印刷プレビュー

反応式

HRID 1271491 の反応式
S([O-])([O-])(=O)=O.[Mg+2].[NH2:7][CH:8]1[CH2:14][CH2:13][CH2:12][CH2:11][N:10]([CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[C:9]1=[O:22].C(N(CC)CC)C.C(=O)C1C=CC=CC=1.C[Si]([N-][Si](C)(C)C)(C)C.[Li+].[CH2:48]([O:55][C:56]1[CH:63]=[CH:62][C:59]([CH2:60]Cl)=[CH:58][CH:57]=1)[C:49]1[CH:54]=[CH:53][CH:52]=[CH:51][CH:50]=1>ClCCl.O1CCCC1>[NH2:7][C:8]1([CH2:60][C:59]2[CH:62]=[CH:63][C:56]([O:55][CH2:48][C:49]3[CH:54]=[CH:53][CH:52]=[CH:51][CH:50]=3)=[CH:57][CH:58]=2)[CH2:14][CH2:13][CH2:12][CH2:11][N:10]([CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[C:9]1=[O:22]
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

9

反応物 6

HCID 240BenzaldehydeHCID 8471TriethylamineHCID 24083Sulfuric acid magnesium salt (1:1)HCID 700424-Benzyloxybenzyl chlorideHCID 2733832Lithium hexamethyldisilazaneHCID 186125993-Amino-1-benzyl-azepan-2-one

生成物 1

HCID 18451909
3-Amino-1-benzyl-3-[4-(benzyloxy)benzyl]azepan-2-one

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

Magnesium sulfate (5.0 g, 41.5 mmol) was added to a solution of commercially available 3-amino-1-benzylazepan-2-one (940 mg, 4.31 mmol), triethylamine (0.60 mL, 4.31 mmol) and benzaldehyde (0.46 mL, 4.52 mmol) in dichloromethane (20 mL). After 18 h, the mixture was filtered and concentrated to give the crude imine. Lithium bis(trimethylsilyl)amide (1M in tetrahydrofuran; 1.42 mL, 1.42 mmol) was added to a solution of the crude imine (363 mg, 1.19 mmol) in tetrahydrofuran (4 mL). After 2 h, the mixture was cooled to 0° C. 4-benzyloxybenzyl chloride (290 mg, 1.24 mmol) was added and the mixture was allowed to warm to ambient temperature. After an additional 18 h, the mixture was quenched with 1N hydrochloric acid (10 mL). After 30 min, the mixture was extracted with ethyl acetate, and the organic layer was washed with aqueous saturated sodium carbonate, water, saturated brine, dried over magnesium sulfate, filtered, and concentrated. Purification by silica gel chromatography [100% dichloromethane→90% dichloromethane/10% methanol (10% ammonium hydroxide/methanol)] gave the title compound. (109 mg) MS 415 (M+1). 1H NMR (500 MHz, CDCl3) δ 7.44–7.36 (m, 4H), 7.34–7.23 (m, 6H), 7.03 (d, J=8.6 Hz, 2H), 6.81 (d, J=8.6 Hz, 2H), 5.29 (s, 2H), 4.64–4.52 (m, 2H), 3.31–3.26 (m, 1H), 3.22–3.18 (m, 1H), 3.02 (d, J=13.4 Hz, 1H), 2.86 (d, J=13.7 Hz, 1H), 1.90–1.75 (m, 4H), 1.72–1.60 (m, 2H), 1.49–1.42 (m, 2H).

後処理

  1. filtrationthe mixture was filtered
  2. concentrationconcentrated
  3. customto give the crude imine
  4. waitAfter 2 h
  5. temperatureto warm to ambient temperature
  6. waitAfter an additional 18 h
  7. customthe mixture was quenched with 1N hydrochloric acid (10 mL)
  8. waitAfter 30 min
  9. extractionthe mixture was extracted with ethyl acetate
  10. washthe organic layer was washed with aqueous saturated sodium carbonate, water, saturated brine
  11. dry with materialdried over magnesium sulfate
  12. filtrationfiltered
  13. concentrationconcentrated
  14. customPurification by silica gel chromatography [100% dichloromethane→90% dichloromethane/10% methanol (10% ammonium hydroxide/methanol)]

出典と根拠

ORDレコード
ord-006ff5c99a9f4ac99f2fab6c0ac6bdb8
出典データセット
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07205292B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート