1,2-Dichloroethane → HCID 178452121、化合物

HRID 659784

反応式

HRID 659784 の反応式
[N+:1]([C:4]1[C:5]([C:9]([OH:11])=O)=[N:6][NH:7][CH:8]=1)([O-:3])=[O:2].[NH2:12][CH:13]1[CH2:18][CH2:17][N:16]([C:19]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20])[CH2:15][CH2:14]1.C(Cl)CCl.C1C=NC2N(O)N=NC=2C=1>CN(C=O)C>[C:22]([O:21][C:19]([N:16]1[CH2:17][CH2:18][CH:13]([NH:12][C:9]([C:5]2[C:4]([N+:1]([O-:3])=[O:2])=[CH:8][NH:7][N:6]=2)=[O:11])[CH2:14][CH2:15]1)=[O:20])([CH3:25])([CH3:23])[CH3:24]

参加物

6

反応物 4

HCID 111,2-DichloroethaneHCID 181649HOAtHCID 12682914-Amino-1-Boc-piperidineHCID 178524956HCID 178524956、化合物

生成物 1

HCID 178452121HCID 178452121、化合物収率 241.9%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

4-Nitropyrazole-3-carboxylic acid (7.3 g; 15.9 mmol) was added to a stirred solution of 4-amino-1-Boc-piperidine (10.2 mg; 51 mmol), EDC (10.7 g; 55.8 mmol), and HOAt (55.8 g; 19.1 mmol) in DMF (100 ml), and then stirred at room temperature overnight. The solvent was removed by evaporation under reduced pressure and the residue triturated with water (250 ml). The resultant cream solid was collected by filtration, washed with water then dried under vacuum to give 13.05 g of 4-[(4-nitro-1H-pyrazole-3-carbonyl)-amino]-piperidine-1-carboxylic acid tert-butyl ester (LC/MS: Rt 2.50, [M+H]+ 340).

後処理

  1. customThe solvent was removed by evaporation under reduced pressure
  2. customthe residue triturated with water (250 ml)
  3. filtrationThe resultant cream solid was collected by filtration
  4. washwashed with water
  5. customthen dried under vacuum

出典と根拠

ORDレコード
ord-96bb0c4c4e224d539215585bbf8e40dc
出典データセット
uspto-grants-2011_12
特許番号
US08080666B2

関連ノート

読み込み中…