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2-Amino-5-chloropyridine → HCID 66705878、化合物

HRID 2276373
ノート
印刷プレビュー

反応式

HRID 2276373 の反応式
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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

10

反応物 6

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

生成物 1

HCID 66705878
HCID 66705878、化合物
収率 38%

試薬・触媒・溶媒 3

HCID 6344Dichloromethane溶媒HCID 63651,1-Dichloroethane溶媒2 回HCID 8471Triethylamine溶媒

反応条件

温度
50 °C

実験手順

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]+).

後処理

  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)

出典と根拠

ORDレコード
ord-e1aa8b0cb4d34d5cb5acc0a7b471a382
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09132136B2

反応ノート

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