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Triethylamine → 1,1-Dimethylethyl (2S)-4-{[4-(acetylamino)-2-methylphenyl]methyl}-2-methyl-1-piperazinecarboxylate

HRID 906373
ノート
印刷プレビュー

反応式

HRID 906373 の反応式
[CH:1]([C:3]1[CH:8]=[CH:7][C:6]([NH:9][C:10](=[O:12])[CH3:11])=[CH:5][C:4]=1[CH3:13])=O.Cl.[CH3:15][C@H:16]1[CH2:21][NH:20][CH2:19][CH2:18][N:17]1[C:22]([O:24][C:25]([CH3:28])([CH3:27])[CH3:26])=[O:23].C(N(CC)CC)C.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C([O-])(O)=O.[Na+]>ClCCCl>[C:10]([NH:9][C:6]1[CH:7]=[CH:8][C:3]([CH2:1][N:20]2[CH2:19][CH2:18][N:17]([C:22]([O:24][C:25]([CH3:28])([CH3:27])[CH3:26])=[O:23])[C@@H:16]([CH3:15])[CH2:21]2)=[C:4]([CH3:13])[CH:5]=1)(=[O:12])[CH3:11]
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 516892Sodium BicarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 12931765N-(4-Formyl-3-methylphenyl)acetamideHCID 45072182(S)-tert-butyl 2-methylpiperazine-1-carboxylate hydrochloride

生成物 1

HCID 59262144
1,1-Dimethylethyl (2S)-4-{[4-(acetylamino)-2-methylphenyl]methyl}-2-methyl-1-piperazinecarboxylate
収率 88.1%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

N-(4-Formyl-3-methylphenyl)acetamide (D52) (326 mg, 1.8 mmol), 1,1-dimethylethyl (2S)-2-methyl-1-piperazinecarboxylate hydrochloride (436 mg, 1.8 mmol), triethylamine (0.282 ml, 2 mmol) and sodium tri(acetoxy)borohydride (781 mg, 3.7 mmol) were stirred together in 1,2-DCE (15 ml) for 17 h. Saturated aqueous NaHCO3 was added and the reaction mixture stirred for 1 h. The organic layer was separated and washed with water and brine, then dried and concentrated to give the crude product which was purified by chromatography. Elution with 0-100% EtOAc/petroleum ether yielded the title compound as a colourless oil (573 mg). δH (CDCl3, 400 MHz) 7.27 (2H, m), 7.16 (1H, d), 7.11 (1H, br.s), 4.17 (1H, m), 3.78 (1H, m), 3.36 (2H, s), 3.02 (1H, m), 2.70 (1H, m), 2.56 (1H, m), 2.36 (3H, s), 2.17 (4H, m), 1.95 (1H, m), 1.45 (9H, s), 1.18 (3H, d). MH+ 362.3.

後処理

  1. customThe organic layer was separated
  2. washwashed with water and brine
  3. customdried
  4. concentrationconcentrated
  5. customto give the crude product which
  6. customwas purified by chromatography
  7. washElution with 0-100% EtOAc/petroleum ether

出典と根拠

ORDレコード
ord-8601780eafde40c6ad2e37010458d0a5
出典データセット
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08012981B2

反応ノート

読み込み中…

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