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2-Amino-5-chloropyridine → HCID 66705878, 화합물

HRID 2276373
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HRID 2276373 반응식
NC1C=CC(Cl)=CN=1.ClC(Cl)(OC(=O)OC(Cl)(Cl)Cl)Cl.[Cl-].C([NH+](CC)CC)C.[Cl:29][C:30]1[CH:31]=[CH:32][C:33]([N:36]=[C:37]=[O:38])=[N:34][CH:35]=1.[NH2:39][C:40]1[CH:45]=[CH:44][C:43]([CH:46]2[CH2:50][CH2:49][N:48]([C:51]([O:53][C:54]([CH3:57])([CH3:56])[CH3:55])=[O:52])[CH2:47]2)=[CH:42][CH:41]=1.C(N(CC)C(C)C)(C)C>ClC(Cl)C.ClCCl.C(N(CC)CC)C>[C:54]([O:53][C:51]([N:48]1[CH2:49][CH2:50][CH:46]([C:43]2[CH:44]=[CH:45][C:40]([NH:39][C:37]([NH:36][C:33]3[CH:32]=[CH:31][C:30]([Cl:29])=[CH:35][N:34]=3)=[O:38])=[CH:41][CH:42]=2)[CH2:47]1)=[O:52])([CH3:57])([CH3:55])[CH3:56]
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참가 물질

10

반응물 6

HCID 661742-Amino-5-chloropyridineHCID 81531DiisopropylethylamineHCID 94429TriphosgeneHCID 12698378Triethylazanium chlorideHCID 205331395-Chloro-2-isocyanatopyridineHCID 57365069Tert-butyl 3-(4-aminophenyl)pyrrolidine-1-carboxylate

생성물 1

HCID 66705878
HCID 66705878, 화합물
수율 38%

시약·촉매·용매 3

HCID 6344Dichloromethane용매HCID 63651,1-Dichloroethane용매2회HCID 8471Triethylamine용매

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온도
50 °C

실험 절차

To a stirred suspension of 2-amino-5-chloro-pyridine (1.01 g) in dichloroethane (20 ml) was added portionwise triphosgene (831 mg). Triethylamine (2.22 ml) was then added dropwise and the mixture was stirred at 50° C. for 1 h. The mixture was then concentrated in vacuo to afford a beige solid containing a mixture of triethylammonium chloride and 5-chloro-2-isocyanato-pyridine. This solid was then added to a stirred solution of (RS)-tert-butyl 3-(4-aminophenyl)pyrrolidine-1-carboxylate (350 mg, CAS 908334-28-1) and N,N-diisopropylethylamine (0.68 ml) in dichloroethane (6 ml) and the resulting mixture was stirred at 60° C. overnight. The mixture was then diluted with dichloromethane and washed with water. The phases were separated and the organic phase was dried over sodium sulphate and concentrated in vacuo. The residue was purified by column chromatography (SiO2; gradient: heptane/EtOAc) to give (RS)-3-{4-[3-(5-chloro-pyridin-2-yl)-ureido]-phenyl}-pyrrolidine-1-carboxylic acid tert-butyl ester (212 mg, 38%) as an off-white solid. MS (ISP): 419.2 ([{37Cl}M+H]+), 417.2 ([{35Cl}M+H]+).

후처리

  1. concentrationThe mixture was then concentrated in vacuo
  2. customto afford a beige solid
  3. additioncontaining
  4. stirringthe resulting mixture was stirred at 60° C. overnight
  5. washwashed with water
  6. customThe phases were separated
  7. dry with materialthe organic phase was dried over sodium sulphate
  8. concentrationconcentrated in vacuo
  9. customThe residue was purified by column chromatography (SiO2; gradient: heptane/EtOAc)

출처 및 근거

ORD 기록
ord-e1aa8b0cb4d34d5cb5acc0a7b471a382
출처 데이터셋
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09132136B2

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