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Water → HCID 178441449, 화합물

HRID 1655448
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HRID 1655448 반응식
[CH2:1]([C:5]1[N:9]([CH2:10][C:11]2[CH:16]=[CH:15][C:14]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=3[C:23]#[N:24])=[CH:13][CH:12]=2)[C:8]2[CH:25]=[CH:26][CH:27]=[CH:28][C:7]=2[N:6]=1)[CH2:2][CH2:3][CH3:4].[N-:29]=[N+:30]=[N-:31].[Na+].[Cl-].[NH4+].O>CN(C=O)C.C(OCC)(=O)C>[CH2:1]([C:5]1[N:9]([CH2:10][C:11]2[CH:16]=[CH:15][C:14]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=3[C:23]3[NH:31][N:30]=[N:29][N:24]=3)=[CH:13][CH:12]=2)[C:8]2[CH:25]=[CH:26][CH:27]=[CH:28][C:7]=2[N:6]=1)[CH2:2][CH2:3][CH3:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 25517Ammonium Chloride2회HCID 33557Sodium Azide2회HCID 197921082-Butyl-1-[(2'-cyanobiphenyl-4-yl)methyl]benzimidazole

생성물 1

HCID 178441449HCID 178441449, 화합물수율 41%

시약·촉매·용매 2

HCID 6228
Dimethylformamide
용매
2회
HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 2-butyl-1-[(2'-cyanobiphenyl-4-yl)methyl]benzimidazole (1.8 g), sodium azide (0.98 g) and ammonium chloride (0.80 g) was stirred in DMF (6 ml) at 110° C. for 5 days, while supplementing sodium azide (1.6 g), ammonium chloride (1.3 g) and DMF (5 ml) to the reaction system. To the reaction mixture were added water and ethyl acetate, and precipitating crystals were collected by filtration. The organic layer of the filtrate was washed with water, dried and concentrated under reduced pressure to give crude crystals. These crystals were combined with the crystals obtained previously, this was followed by recrystallization from ethyl acetate - methanol to afford colorless prisms (0.82 g, 41%), m.p. 235-236° C.

후처리

  1. customprecipitating crystals
  2. filtrationwere collected by filtration
  3. washThe organic layer of the filtrate was washed with water
  4. customdried
  5. concentrationconcentrated under reduced pressure
  6. customto give crude crystals
  7. customobtained previously
  8. customthis was followed by recrystallization from ethyl acetate - methanol

출처 및 근거

ORD 기록
ord-3ae554d6481c4bb7bff7dc0396bb5543
출처 데이터셋
uspto-grants-1993_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05250554

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