Sodium Carbonate → HCID 53952014、化合物

HRID 1533993ノート

反応式

HRID 1533993 の反応式
[CH3:1][C:2]([NH:5][CH2:6][CH2:7][CH2:8][O:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[C:16]([C:18]1[CH:26]=[CH:25][CH:24]=[C:23]2[C:19]=1[CH:20]=[CH:21][NH:22]2)=[O:17])([CH3:4])[CH3:3].[Cl:27]N1C(=O)CCC1=O.C(=O)([O-])[O-].[Na+].[Na+]>C(O)(=O)C>[CH3:4][C:2]([NH:5][CH2:6][CH2:7][CH2:8][O:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[C:16]([C:18]1[CH:26]=[CH:25][CH:24]=[C:23]2[C:19]=1[C:20]([Cl:27])=[CH:21][NH:22]2)=[O:17])([CH3:1])[CH3:3]

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 31398ChlorosuccinimideHCID 3077190HCID 3077190、化合物

生成物 1

HCID 53952014HCID 53952014、化合物収率 79.8%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

6.3 g of [2-[3-[(1,1-dimethylethyl)-amino]-propoxy]-phenyl]-(1H-indol-4-yl) methanone of Step F of Example 3 in 50 ml of acetic acid in the presence of 2.64 g of N-chloro succinimide was stirred for 2 hours at ambient temperature and was then poured into 300 ml of saturated aqueous solution of sodium carbonate and extracted with ethyl acetate. The organic phase was washed with salt water, dried and concentrated to dryness. After chromatography of the residue on silica (eluant:ethyl acetate triethylamine 95-5), 5.52 g of the expected product were obtained and was used as is for the following step.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe organic phase was washed with salt water
  3. customdried
  4. concentrationconcentrated to dryness

出典と根拠

ORDレコード
ord-7aea540fc66f40bcbe03944dcba89d2b
出典データセット
uspto-grants-1992_02
特許番号
US05086070

反応ノート

読み込み中…