Thiabendazole → HCID 21441751, 화합물

HRID 328339노트

반응식

HRID 328339 반응식
Cl[C:2]([O:4][CH2:5][CH2:6][CH:7]([CH2:9][CH2:10][CH:11]=[C:12]([CH3:14])[CH3:13])[CH3:8])=[O:3].[S:15]1[CH:19]=[C:18]([C:20]2[NH:21][C:22]3[CH:28]=[CH:27][CH:26]=[CH:25][C:23]=3[N:24]=2)[N:17]=[CH:16]1>N1C=CC=CC=1>[CH2:5]([O:4][C:2]([N:24]1[C:23]2[CH:25]=[CH:26][CH:27]=[CH:28][C:22]=2[N:21]=[C:20]1[C:18]1[N:17]=[CH:16][S:15][CH:19]=1)=[O:3])[CH2:6][CH:7]([CH2:9][CH2:10][CH:11]=[C:12]([CH3:14])[CH3:13])[CH3:8]

참가 물질

4

반응물 2

HCID 5430ThiabendazoleHCID 185209753,7-Dimethyloct-6-en-1-yl carbonochloridate

생성물 1

HCID 21441751HCID 21441751, 화합물수율 86.6%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

11.0 Grams (0.05 moles) of citronellyl chloroformate is added over a period of 1/2 hour to a stirred suspension of 10 grams (0.05 moles) of 2-(4-thiazolyl)benzimidazole and 75 ml. of pyridine at room temperature. The reaction mixture is stirred overnight at room temperature protected from moisture. The solid material is filtered, washed with pryidine and the filtrate and washings evaporated to dryness in vacuo. The residue is dissolved in methylene chloride and the solution washed successively with dilute cold hydrochloric acid, cold water, cold dilute sodium bicarbonate solution and water. The methylene chloride is dried, evaporated to dryness in vacuo affording 16.6 grams of a viscous oil. The oil is chromatographed on a column of silica gel eluting with hexane affording 14.6 grams (76%) of an oil which thin layer chromatography reveals to be pure material and which analyzes as 1-citronellyloxycarbonyl-2-(4-thiazolyl)benzimidazole.

후처리

  1. customat room temperature
  2. filtrationThe solid material is filtered
  3. washwashed with pryidine
  4. customthe filtrate and washings evaporated to dryness in vacuo
  5. dissolutionThe residue is dissolved in methylene chloride
  6. washthe solution washed successively
  7. additionwith dilute cold hydrochloric acid, cold water, cold dilute sodium bicarbonate solution and water
  8. dry with materialThe methylene chloride is dried
  9. customevaporated to dryness in vacuo

출처 및 근거

ORD 기록
ord-2205d1f6cbe2457d89d577609226fe36
출처 데이터셋
uspto-grants-1977_04
특허 번호
US04017505

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