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Methylamine → 1-benzyl-N-methylpiperidine-4-carboxamide

HRID 1351416
ノート
印刷プレビュー

反応式

HRID 1351416 の反応式
[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([C:14]([OH:16])=O)[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.[CH3:18][N:19](C)CCCN=C=NCC.O.ON1C2C=CC=CC=2N=N1.CN>O1CCCC1.ClCCl>[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([C:14]([NH:19][CH3:18])=[O:16])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=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 4

HCID 6329MethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 47149831-Benzylpiperidine-4-carboxylic acid

生成物 1

HCID 409218631-benzyl-N-methylpiperidine-4-carboxamide

試薬・触媒・溶媒 2

HCID 6344
Dichloromethane
溶媒
HCID 8028Tetrahydrofuran溶媒

実験手順

N-Benzyl 4-piperidinecarboxylic acid (5.00 g, 22.8 mmol), 1-(3-dimethylaminopropyl)-3-ethyl-carbodiimide hydrochloride (5.25 g, 27.4 mmol) and 1-hydroxybenzotriazole hydrate (3.84 g, 25.1 mmol) were added to a solution of methylamine (11.4 ml of a 2.0M solution in tetrahydrofuran, 22.8 mmol) in dichloromethane (100 ml). The mixture was stirred for 1 hour at room temperature, then partitioned between dichloromethane and water. The organic layer was separated and washed with brine, dried (MgSO4), filtered and evaporated under reduced pressure to furnish a pale yellow solid, 3.50 g.

後処理

  1. custompartitioned between dichloromethane and water
  2. customThe organic layer was separated
  3. washwashed with brine
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. customevaporated under reduced pressure
  7. customto furnish a pale yellow solid, 3.50 g

出典と根拠

ORDレコード
ord-c98c2f2415ae45c6a251024ef89a28d6
出典データセット
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07217714B1

反応ノート

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