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1-Bromooctane → HCID 178443879, 화합물

HRID 1030579
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HRID 1030579 반응식
[Cl:1][C:2]1[CH:11]=[CH:10][C:5]2[N:6]=[C:7]([SH:9])[NH:8][C:4]=2[CH:3]=1.[OH-].[Na+].[CH2:14](Br)[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH3:21]>CO>[Cl:1][C:2]1[CH:11]=[CH:10][C:5]2[NH:6][C:7]([S:9][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH3:21])=[N:8][C:4]=2[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 81401-BromooctaneHCID 14798Sodium HydroxideHCID 178527787HCID 178527787, 화합물

생성물 1

HCID 178443879HCID 178443879, 화합물수율 75.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 5-chloro-2-mercaptobenzimidazole (1.84 c, 10 mmol) (Varima, R. S., J. Indian Chem. Soc. 62, 73 (1985)) in methanol (10 mL) and 2N sodium hydroxide (13 mmol) was added octyl bromide (2.17 g, 10 mmol). The solution was stirred at ambient temperature for 72 hours, evaporated, dissolved in CH2Cl2, washed with brine and dried over Na2SO4. Evaporation of the solvent and flash chromatography (Merck Kieselgel, 5% Et2O/CH2Cl2) gave a residue which solidified on standing. A pentane wash gave the title compound as a beige solid (2.23 g), m.p. 66°-67° C. NMR (CDCl3)δ7.3(m, 3H), 5.33(t, J=6 Hz, 2H), 1.20(br, 15H).

후처리

  1. customevaporated
  2. dissolutiondissolved in CH2Cl2
  3. washwashed with brine
  4. dry with materialdried over Na2SO4
  5. customEvaporation of the solvent and flash chromatography (Merck Kieselgel, 5% Et2O/CH2Cl2)
  6. customgave a residue which
  7. washA pentane wash

출처 및 근거

ORD 기록
ord-e9d6bf8e10f34d2496191bbd7b15463c
출처 데이터셋
uspto-grants-1992_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05106863

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