Sodium Hydroxide → HCID 20324952, 화합물

HRID 838855노트

반응식

HRID 838855 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 20324952HCID 20324952, 화합물수율 76.8%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-97b69ec5311349f7bc3f44710ecb64a4
출처 데이터셋
uspto-grants-1978_06
특허 번호
US04093617

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