Ethanol → 5-azido-1,2,7-trimethyl-1H-benzimidazole

HRID 1846438노트

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HRID 1846438 반응식
Br[C:2]1[CH:12]=[C:11]([CH3:13])[C:5]2[N:6]([CH3:10])[C:7]([CH3:9])=[N:8][C:4]=2[CH:3]=1.[N-:14]=[N+:15]=[N-:16].[Na+].[Na].O=C1O[C@H]([C@H](CO)O)C(O)=C1O.C(O)C>[Cu]I.O>[N:14]([C:2]1[CH:12]=[C:11]([CH3:13])[C:5]2[N:6]([CH3:10])[C:7]([CH3:9])=[N:8][C:4]=2[CH:3]=1)=[N+:15]=[N-:16]

참가 물질

7

반응물 4

HCID 702EthanolHCID 33557Sodium AzideHCID 66586226sodium L-ascorbic acidHCID 669781805-bromo-1,2,7-trimethyl-1H-benzimidazole

생성물 1

HCID 866638995-azido-1,2,7-trimethyl-1H-benzimidazole

시약·촉매·용매 2

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)촉매HCID 962Water용매

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온도
100 °C

실험 절차

0.59 g (2.50 mmol) 5-bromo-1,2,7-trimethyl-1H-benzimidazole, 0.32 g (4.9 mmol) sodium azide, 75 mg (0.50 mmol) trans-(1R,2R)—N,N′-bismethyl-1,2-cyclohexane-diamine, 50 mg (0.30 mmol) copper(I) iodide and 50 mg (0.30 mmol) L-ascorbic acid sodium salt were added to 2.0 ml of a mixture of ethanol and water (EtOH/water=7/3) and the mixture was stirred for 1 h at 100° C. Then the EtOH was distilled off and the residue was mixed with water. The precipitate formed was suction filtered, washed with water and diethyl ether and dried.

후처리

  1. distillationThen the EtOH was distilled off
  2. additionthe residue was mixed with water
  3. customThe precipitate formed
  4. filtrationfiltered
  5. washwashed with water and diethyl ether
  6. customdried

출처 및 근거

ORD 기록
ord-68f560f4790a4abab2c43fd861bc7808
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08952014B2

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