Water → HCID 86593419、化合物

HRID 1247847ノート

反応式

HRID 1247847 の反応式
[NH2:1][C:2]1[N:6]([CH2:7][CH2:8][F:9])[N:5]=[CH:4][C:3]=1[NH:10][C:11](=[O:22])[CH2:12][CH2:13][NH:14][C:15](=[O:21])[O:16][C:17]([CH3:20])([CH3:19])[CH3:18].C(N(CC)CC)C.[C:30](Cl)([C:43]1[CH:48]=[CH:47][CH:46]=[CH:45][CH:44]=1)([C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1)[C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1.O>CN(C)C=O.CN(C)C1C=CN=CC=1>[F:9][CH2:8][CH2:7][N:6]1[C:2]([NH:1][C:30]([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)([C:43]2[CH:44]=[CH:45][CH:46]=[CH:47][CH:48]=2)[C:37]2[CH:38]=[CH:39][CH:40]=[CH:41][CH:42]=2)=[C:3]([NH:10][C:11](=[O:22])[CH2:12][CH2:13][NH:14][C:15](=[O:21])[O:16][C:17]([CH3:19])([CH3:18])[CH3:20])[CH:4]=[N:5]1

参加物

7

反応物 4

HCID 962WaterHCID 6456Trityl chlorideHCID 8471TriethylamineHCID 86593418HCID 86593418、化合物

生成物 1

HCID 86593419HCID 86593419、化合物収率 49.2%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6228Dimethylformamide溶媒

実験手順

To a solution of tert-butyl (3-{[5-amino-1-(2-fluoroethyl)-1H-pyrazol-4-yl]amino}-3-oxopropyl)carbamate (2.3 g) in N,N-dimethylformamide (12 ml) were added triethylamine (1.48 g), 4-dimethylaminopyridine (35.6 mg) and trityl chloride (2.2 g) at room temperature. The reaction mixture was stirred for 2 hours, and water was added. The mixture was extracted with ethyl acetate, and the organic layer was washed with water and aqueous sodium chloride solution. The organic layer was dried over magnesium sulfate and concentrated in vacuo. Acetonitrile was added, and the precipitate was collected by filtration to give tert-butyl (3-{[1-(2-fluoroethyl)-5-(tritylamino)-1H-pyrazol-4-yl]amino}-3-oxopropyl)carbamate (2 g).

後処理

  1. extractionThe mixture was extracted with ethyl acetate
  2. washthe organic layer was washed with water and aqueous sodium chloride solution
  3. dry with materialThe organic layer was dried over magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. additionAcetonitrile was added
  6. filtrationthe precipitate was collected by filtration

出典と根拠

ORDレコード
ord-9ead8a85dc9547ce8bf9d5cf91bdf0e7
出典データセット
uspto-grants-2006_10
特許番号
US07129232B2

反応ノート

読み込み中…