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Water → HCID 178476553, 화합물

HRID 415123
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HRID 415123 반응식
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([CH2:8][CH2:9][CH2:10][O:11][C:12]2[CH:13]=[C:14]([NH2:19])[C:15]([NH2:18])=[CH:16][CH:17]=2)[CH2:4][CH2:3]1.[OH2:20].[N:21]#[C:22]Br>C(O)(=O)C>[C:12]([OH:20])(=[O:11])[CH3:13].[C:10]([OH:11])(=[O:20])[CH3:9].[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([CH2:8][CH2:9][CH2:10][O:11][C:12]2[CH:17]=[CH:16][C:15]3[NH:18][C:22]([NH2:21])=[N:19][C:14]=3[CH:13]=2)[CH2:4][CH2:3]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 10476Cyanogen BromideHCID 59349505HCID 59349505, 화합물

생성물 1

HCID 178476553HCID 178476553, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A 100 mL flasked was charged with 4-(3-(4-methylpiperazin-1-yl)propoxy)benzene-1,2-diamine (1.15 g, 4.35 mmol), water (50 mL) and acetic acid (2 mL) and stirred at room temperature for 15 minutes. The reaction mixture was placed in an ice bath and then charged with cyanogen bromide (0.526 g, 5 mmol). The reaction mixture was allowed to warm to room temperature and stirred over night. The reaction mixture was concentrated under reduced pressure and redissolved in acetone, dried over anhydrous sodium sulfate, and then filtered. The filtrate was concentrated under reduced pressure to give 1.7 g of 5-(3-(4-methylpiperazin-1-yl)propoxy)-1H-benzo[d]imidazol-2-amine diacetate. This material was used without any further purification. MS (EI): 290 (MH+).

후처리

  1. customThe reaction mixture was placed in an ice bath
  2. temperatureto warm to room temperature
  3. stirringstirred over night
  4. concentrationThe reaction mixture was concentrated under reduced pressure
  5. dissolutionredissolved in acetone
  6. dry with materialdried over anhydrous sodium sulfate
  7. filtrationfiltered
  8. concentrationThe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-8349770d12d14de29e2ced74af3b71c4
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08088767B2

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