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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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HCID 86630875, 화합물 → 4,5-Diamino-6-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]-2-methylbiphenyl-3-carbonitrile

HRID 17554
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HRID 17554 반응식
[NH2:1][C:2]1[C:7]([N+:8]([O-])=O)=[C:6]([N:11]2[CH2:15][CH2:14][C@H:13]([N:16]([CH3:18])[CH3:17])[CH2:12]2)[C:5]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[C:4]([CH3:25])[C:3]=1[C:26]#[N:27]>O.O.O.O.O.O.[Fe](Cl)Cl.[Zn].CN(C)C=O>[NH2:1][C:2]1[C:7]([NH2:8])=[C:6]([N:11]2[CH2:15][CH2:14][C@H:13]([N:16]([CH3:17])[CH3:18])[CH2:12]2)[C:5]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[C:4]([CH3:25])[C:3]=1[C:26]#[N:27]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 1

HCID 86630875HCID 86630875, 화합물

생성물 1

HCID 866308764,5-Diamino-6-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]-2-methylbiphenyl-3-carbonitrile수율 97.3%

시약·촉매·용매 3

HCID 23994Zinc촉매HCID 129819097HCID 129819097, 화합물촉매HCID 6228Dimethylformamide용매

실험 절차

An aqueous solution (14 ml) of iron chloride hexahydrate (0.83 g, 3.06 mmol) and zinc (5.01 g, 76.6 mmol) were added to an N,N-dimethylformamide (35 ml) solution of 4-amino-6-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]-2-methyl-5-nitrobiphenyl-3-carbonitrile (I-268) (1.40 g, 3.83 mmol), followed by stirring at room temperature for 1 hour. The insoluble matter was removed by filtration under suction, then the filtrate was diluted with ethyl acetate, washed with aqueous saturated sodium carbonate solution and saturated brine in that order, and dried over anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure, followed by drying with a vacuum pump to obtain the entitled compound (1.25 g, 97%) as a dark brown solid.

후처리

  1. customThe insoluble matter was removed by filtration under suction
  2. additionthe filtrate was diluted with ethyl acetate
  3. washwashed with aqueous saturated sodium carbonate solution and saturated brine in that order
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent was evaporated away under reduced pressure
  6. customby drying with a vacuum pump

출처 및 근거

ORD 기록
ord-1a0f2bcf5dc94f82a80cbefce8556a45
출처 데이터셋
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07737166B2

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