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Phosgene → (3S-trans)-N-[[3-[[t-Butoxycarbonyl]amino]-4-methyl-2-oxo-1-azetidinyl]carbonyl]-N-methylglycine, t-butyl ester

HRID 482926
ノート
印刷プレビュー

反応式

HRID 482926 の反応式
[C:1](Cl)(Cl)=[O:2].[CH3:5][NH:6][CH2:7][C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9].C(N(CC)CC)C.[C:22]([O:26][C:27]([NH:29][C@H:30]1[C@H:33]([CH3:34])[NH:32][C:31]1=[O:35])=[O:28])([CH3:25])([CH3:24])[CH3:23]>C1(C)C=CC=CC=1.ClCCl.C(OCC)(=O)C>[C:22]([O:26][C:27]([NH:29][C@H:30]1[C@H:33]([CH3:34])[N:32]([C:31]([N:6]([CH3:5])[CH2:7][C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])=[O:35])[C:1]1=[O:2])=[O:28])([CH3:25])([CH3:24])[CH3:23]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 6371PhosgeneHCID 8471Triethylamine3 回HCID 5069406Tert-butyl 2-(methylamino)acetateHCID 13155285tert-Butyl ((2S,3S)-2-methyl-4-oxoazetidin-3-yl)carbamate

生成物 1

HCID 131714548(3S-trans)-N-[[3-[[t-Butoxycarbonyl]amino]-4-methyl-2-oxo-1-azetidinyl]carbonyl]-N-methylglycine, t-butyl ester

試薬・触媒・溶媒 3

HCID 1140
Toluene
溶媒
HCID 6344Dichloromethane溶媒2 回
HCID 8857Ethyl Acetate溶媒

実験手順

A solution of phosgene in toluene (1.35 ml of a 20% solution, 2.698 mmol) was cooled to -25° C. under an argon atmosphere. A solution of N-methylglycine, t-butyl ester (218 mg, 1.498 mmol) and triethylamine (251 μl, 1.798 mmol) in dichloromethane (2 ml) was added dropwise over 5 minutes. The reaction was stirred for 1 hour at -25° C. (after 15 minutes an additional 0.2 ml of dichloromethane was added to facilitate stirring). The volatiles were removed starting at -25° C. and slowly by warming to room temperature. The residue was dissolved in methylene chloride (5 ml), cooled to 0° C. and treated with (3S-trans)-3-[[t-butoxycarbonyl]amino]-4-methyl-2-azetidinone (300 mg, 1.498 mmol; pre-dried over P2O5 at 25° C. under high vacuum), 4-dimethylaminiopyridine (18 mg, 0.149 mmol), and triethylamine (251 μl, 1.798 mmol). The resulting mixture was warmed to room temperature, stirred for 36 hours, treated with additional triethylamine (502 μl), and refluxed for 5 hours. The reaction was cooled, diluted with ethyl acetate, washed with pH 4.5 KH2PO4, and with brine, and then dried over sodium sulfate. Filtration and concentration in vacuo produced 525 mg of an oil which was chromatographed on 21 g of silica gel (230-400 mesh). Elution with 40% ethyl acetate-hexane gave 356 mg of the title compound as a white solid.

後処理

  1. additionwas added
  2. customThe volatiles were removed
  3. customstarting at -25° C.
  4. dissolutionThe residue was dissolved in methylene chloride (5 ml)
  5. temperaturecooled to 0° C.
  6. temperatureThe resulting mixture was warmed to room temperature
  7. stirringstirred for 36 hours
  8. temperaturerefluxed for 5 hours
  9. temperatureThe reaction was cooled
  10. washwashed with pH 4.5 KH2PO4
  11. dry with materialwith brine, and then dried over sodium sulfate
  12. filtrationFiltration and concentration in vacuo

出典と根拠

ORDレコード
ord-25da6eb50cac4975a77a2a733776fabe
出典データセット
uspto-grants-1986_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04576749

反応ノート

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