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Triethylamine → benzyl((1R,2S)-2-{[((2RS)-6-fluoro-1,2,3,4-tetrahydronaphthalen-2-yl)amino]methyl}cyclohexyl)carbamate

HRID 1592337
ノート
印刷プレビュー

反応式

HRID 1592337 の反応式
Cl.[F:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[CH2:9][CH:8]([NH2:13])[CH2:7][CH2:6]2.[CH:14]([C@@H:16]1[CH2:21][CH2:20][CH2:19][CH2:18][C@H:17]1[NH:22][C:23](=[O:32])[O:24][CH2:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)=O.C(N(CC)CC)C.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].[OH-].[Na+]>ClCCCl>[CH2:25]([O:24][C:23](=[O:32])[NH:22][C@@H:17]1[CH2:18][CH2:19][CH2:20][CH2:21][C@H:16]1[CH2:14][NH:13][CH:8]1[CH2:7][CH2:6][C:5]2[C:10](=[CH:11][CH:12]=[C:3]([F:2])[CH:4]=2)[CH2:9]1)[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 5049666Sodium triacetoxyborohydrideHCID 196993636-Fluoro-1,2,3,4-tetrahydro-naphthalen-2-ylamine hydrochlorideHCID 29923903Benzyl [(1r,2r)-2-formylcyclohexyl]carbamate

生成物 1

HCID 131726668
benzyl((1R,2S)-2-{[((2RS)-6-fluoro-1,2,3,4-tetrahydronaphthalen-2-yl)amino]methyl}cyclohexyl)carbamate
収率 69%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

A mixture of (RS)-(6-fluoro-1,2,3,4-tetrahydronaphthalen-2-yl)amine hydrochloride (200 mg, 0.99 mmol) and benzyl [(1R,2R)-2-formylcyclohexyl]carbamate (258 mg, 0.99 mmol) in 1,2-dichloroethane (4 mL) was treated with triethylamine (275 μL, 1.98 mmol) whereupon a clear solution resulted. Sodium triacetoxyborohydride (272 mg, 1.28 mmol) was added and the mixture was stirred at room temperature for 3.5 hours. Aqueous sodium hydroxide (1.0 N) was then added, and the mixture was extracted with ether. The organic phase was dried over sodium sulfate and concentrated. The residue was purified by flash column chromatography, eluting with 5% methanol in dichloromethane, containing 0.5% aqueous ammonia, to provide a colorless oil (280 mg, 69%).

後処理

  1. customresulted
  2. extractionthe mixture was extracted with ether
  3. dry with materialThe organic phase was dried over sodium sulfate
  4. concentrationconcentrated
  5. customThe residue was purified by flash column chromatography
  6. washeluting with 5% methanol in dichloromethane
  7. additioncontaining 0.5% aqueous ammonia

出典と根拠

ORDレコード
ord-4ad87b87e83a4e578a618c6ed8b3d526
出典データセット
uspto-grants-2007_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07291744B2

反応ノート

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