Triethylamine → 3-Oxo-3-[N'-(3,4,5,6-tetrahydro-2H-[1,2']bipyridinyl-4-carbonyl)-hydrazino]-propionic acid tert-butyl ester

HRID 6916

反応式

HRID 6916 の反応式
NN.[C:3]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])(=[O:8])[CH2:4][C:5]([O-:7])=O.[OH2:14].O[N:16]1[C:20]2[CH:21]=CC=CC=2N=[N:17]1.[CH2:25]([N:27]([CH2:30][CH3:31])[CH2:28][CH3:29])[CH3:26].Cl.CN(C)[CH2:35][CH2:36][CH2:37][N:38]=C=NCC>ClCCl>[C:10]([O:9][C:3](=[O:8])[CH2:4][C:5](=[O:7])[NH:17][NH:16][C:20]([CH:21]1[CH2:29][CH2:28][N:27]([C:30]2[CH:31]=[CH:35][CH:36]=[CH:37][N:38]=2)[CH2:25][CH2:26]1)=[O:14])([CH3:13])([CH3:12])[CH3:11]

参加物

7

反応物 5

HCID 8471TriethylamineHCID 9321HydrazineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 21883978Tert-butyl malonate

生成物 1

HCID 235440723-Oxo-3-[N'-(3,4,5,6-tetrahydro-2H-[1,2']bipyridinyl-4-carbonyl)-hydrazino]-propionic acid tert-butyl ester

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A mixture of the hydrazine from preparation 35 (2.2 g, 10 mmol), tert-butyl malonate (1.6 g, 10 mmol), 1-hydroxybenzotriazole hydrate (2.02 g, 15 mmol), triethylamine (4.8 ml, 20 mmol) and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (2.4 g, 12.5 mmol) in dichloromethane (50 ml) was stirred at room temperature for 5 hours. The reaction was diluted with dichloromethane (200 ml), washed with water (150 ml), dried (MgSO4) and evaporated under reduced pressure. The residual oil was purified by column chromatography on silica gel using ethyl acetate as eluant to afford the title compound, as a white solid, 1.4 g.

後処理

  1. washwashed with water (150 ml)
  2. dry with materialdried (MgSO4)
  3. customevaporated under reduced pressure
  4. customThe residual oil was purified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-2ff387fd184f4f2e8c6f2f73124e8925
出典データセット
uspto-grants-2006_08
特許番号
US07084145B2

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