Sodium Hydroxide → HCID 20324952、化合物

HRID 838855ノート

反応式

HRID 838855 の反応式
[CH2:1]([C:5]1[CH:10]=[C:9]([CH2:11][CH2:12][CH2:13][CH3:14])[N:8]2[N:15]=[CH:16][CH:17]=[C:7]2[N:6]=1)[CH2:2][CH2:3][CH3:4].[Br:18]N1C(=O)CCC1=O.[OH-].[Na+]>C(Cl)(Cl)Cl>[Br:18][C:17]1[CH:16]=[N:15][N:8]2[C:9]([CH2:11][CH2:12][CH2:13][CH3:14])=[CH:10][C:5]([CH2:1][CH2:2][CH2:3][CH3:4])=[N:6][C:7]=12

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 67184N-bromobutanimideHCID 203249445,7-Dibutylpyrazolo[1,5-a]pyrimidine

生成物 1

HCID 20324952HCID 20324952、化合物収率 76.8%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

A solution of 7.0 g (0.03 mol) of 5,7-di-n-butylpyrazolo[1,5-a]-pyrimidine in 75 ml chloroform was treated with 5.8 g (0.035 mol) of N-bromosuccinimide at room temperature. The mixture was stirred for 5-10 minutes, then poured into ice water, made alkaline with 6N NaOH, and the organic layer separated and dried (Na2SO4). The chloroform solution was chromatographed on neutral alumina (Woelm, grade I) with chloroform as the eluant. Evaporation of the solvent and recrystallization from ligroine gave 7.15 g (72%) of the product, mp 47°-48° C.

後処理

  1. customthe organic layer separated
  2. dry with materialdried (Na2SO4)
  3. customThe chloroform solution was chromatographed on neutral alumina (Woelm, grade I) with chloroform as the eluant
  4. customEvaporation of the solvent and recrystallization from ligroine

出典と根拠

ORDレコード
ord-97b69ec5311349f7bc3f44710ecb64a4
出典データセット
uspto-grants-1978_06
特許番号
US04093617

反応ノート

読み込み中…