Nitrogen → 475648-88-5

HRID 1796338노트

반응식

HRID 1796338 반응식
N#N.[Cl:3][CH2:4][C:5]1[NH:6][C:7]2[CH:13]=[CH:12][CH:11]=[CH:10][C:8]=2[N:9]=1.[H-].[Na+]>C1COCC1>[N:6]1[C:7]2[CH:13]=[CH:12][CH:11]=[CH:10][C:8]=2[NH:9][C:5]=1[CH2:4][N:9]1[C:8]2[CH:10]=[CH:11][CH:12]=[CH:13][C:7]=2[N:6]=[C:5]1[CH2:4][Cl:3]

참가 물질

5

반응물 3

HCID 947NitrogenHCID 24758Sodium hydrideHCID 785712-Chloromethylbenzimidazole

생성물 1

HCID 22181906475648-88-5수율 22,165.699%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a three-necked, 12 L flask, flushed with N2, 2-(chloromethyl)benzimidazole (75 g, 0.45 mmol) and THF (10 L) were added, and the slurry was stirred for one hour at room temperature. Using an ice bath, the slurry was cooled to 0° C. and NaH (5.7 g, 95%, 0.23 mmol) was added. The slurry temperature increased to 4.5° C. The reaction mixture was stirred for 3 h and quenched with 150 g of silica gel. The slurry was concentrated to dryness under reduced pressure and purified using column chromatography (loaded with 40% EtOAc/hexanes, the eluting solvent started with 40% EtOAc/hexanes to end with 75% EtOAc/hexanes). 14.8 g of 1-benzimidazolylmethyl-2-(chloromethyl)benzimidazole 1 was obtained.

후처리

  1. additionwere added
  2. temperaturethe slurry was cooled to 0° C.
  3. temperatureThe slurry temperature increased to 4.5° C
  4. stirringThe reaction mixture was stirred for 3 h
  5. customquenched with 150 g of silica gel
  6. concentrationThe slurry was concentrated to dryness under reduced pressure
  7. custompurified

출처 및 근거

ORD 기록
ord-4a5619eda8944e29b6f60d472242921a
출처 데이터셋
uspto-grants-2006_04
특허 번호
US07030150B2

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