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1,2-Dichloroethane → HCID 69936757, 화합물

HRID 1623780
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HRID 1623780 반응식
[CH:1]1[CH:2]=C[C:4]2[N:9](O)N=[N:7][C:5]=2[CH:6]=1.[CH3:11][N:12]([CH3:32])[C:13]([C:15]1[CH:16]=[CH:17][C:18]([O:24][CH2:25][C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)=[C:19]([CH:23]=1)[C:20]([OH:22])=O)=[O:14].N1C=CC=C(N)C=1.C(Cl)CCl>CN(C)C=O.O>[CH3:32][N:12]([CH3:11])[C:13]([C:15]1[CH:16]=[CH:17][C:18]([O:24][CH2:25][C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)=[C:19]([C:20]([NH:7][C:5]2[CH:4]=[N:9][CH:2]=[CH:1][CH:6]=2)=[O:22])[CH:23]=1)=[O:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 111,2-DichloroethaneHCID 100093-AminopyridineHCID 757711-HydroxybenzotriazoleHCID 67106993HCID 67106993, 화합물

생성물 1

HCID 69936757HCID 69936757, 화합물

시약·촉매·용매 2

HCID 962Water용매
HCID 6228
Dimethylformamide
용매

실험 절차

HOBT (102 mg, 0.67 mmol) was added in one charge to a stirred solution of 5-[(dimethylamino)carbonyl]-2-[(phenylmethyl)oxy]benzoic acid (may be prepared as described in Description 59; 200 mg, 0.67 mmol), 3-pyridinamine (62.9 mg, 0.67 mmol) and EDC (128 mg, 0.67 mmol) in N,N-dimethylformamide (5 ml) under nitrogen at room temperature. The reaction mixture was stirred at room temperature for 4 h. The mixture was diluted with water (50 ml). The precipitate was collected by filtration. The solid was dissolved in ethyl acetate (100 ml), and the organic phase was washed with NaOH (1 mol/l 25 ml), water (25 ml), saturated brine (25 ml), dried over sodium sulfate, and evaporated in vacuo to yield the title compound as a white solid. 78 mg.

후처리

  1. filtrationThe precipitate was collected by filtration
  2. dissolutionThe solid was dissolved in ethyl acetate (100 ml)
  3. washthe organic phase was washed with NaOH (1 mol/l 25 ml), water (25 ml), saturated brine (25 ml)
  4. dry with materialdried over sodium sulfate
  5. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-9d148bd02f994cab8908feea5236dd69
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08778939B2

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