Nitrogen → 475648-88-5

HRID 1796338ノート

反応式

HRID 1796338 の反応式
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]

参加物

5

反応物 3

HCID 947NitrogenHCID 24758Sodium hydrideHCID 785712-Chloromethylbenzimidazole

生成物 1

HCID 22181906475648-88-5収率 22,165.699%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4a5619eda8944e29b6f60d472242921a
出典データセット
uspto-grants-2006_04
特許番号
US07030150B2

反応ノート

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