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Hydrochloric Acid → HCID 178441455, 화합물

HRID 1655479
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인쇄 미리보기

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HRID 1655479 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[C:25]([CH3:29])=[CH:26][CH:27]=[CH:28][C:7]=2[N:6]=1)[CH2:2][CH2:3][CH3:4].[N-:30]=[N+:31]=[N-:32].[Na+].[Cl-].[NH4+].Cl>CN(C=O)C.O>[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:32][N:31]=[N:30][N:24]=3)=[CH:13][CH:12]=2)[C:8]2[C:25]([CH3:29])=[CH:26][CH:27]=[CH:28][C:7]=2[N:6]=1)[CH2:2][CH2:3][CH3:4]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 19792145HCID 19792145, 화합물

생성물 1

HCID 178441455HCID 178441455, 화합물

시약·촉매·용매 2

HCID 962Water용매
HCID 6228
Dimethylformamide
용매

반응 조건

온도
115 °C

실험 절차

A mixture of 2-butyl-1-[(2'-cyanobiphenyl-4-yl)methyl]-7-methylbenzimidazole (0,5 g), sodium azide (1.3 g) and ammonium chloride (1.1 g) in DMF (5 ml) was stirred for 3.5 days at 110-120° C. To the reaction mixture was added water, which was made acidic (pH 3-4) with 1N-HCl, followed by extraction with ethyl acetate. The organic layer was washed with water and dried. The solvent was distilled off, and the residue was purified by column chromatography on silica gel to give crystals. Recrystallization from ethyl acetate-methanol afforded colorless crystals (0.36 g, 62%),

후처리

  1. extractionfollowed by extraction with ethyl acetate
  2. washThe organic layer was washed with water
  3. customdried
  4. distillationThe solvent was distilled off
  5. customthe residue was purified by column chromatography on silica gel
  6. customto give crystals
  7. customRecrystallization from ethyl acetate-methanol afforded colorless crystals (0.36 g, 62%)

출처 및 근거

ORD 기록
ord-49811bd16a82404d9e36a0d9b0b39a45
출처 데이터셋
uspto-grants-1993_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05250554

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