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Toluene → (S)-1-[[3-[[(Phenylmethoxy)carbonyl]amino]-2-oxo-1-azetidinyl]carbonyl]-D-proline, phenylmethyl ester

HRID 482928
ノート
印刷プレビュー

反応式

HRID 482928 の反応式
[NH:1]1[CH2:15][CH2:14][CH2:13][CH:2]1[C:3]([O:5][CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)=[O:4].C(N(CC)CC)C.[C:23](Cl)(Cl)=[O:24].C1(C)C=CC=CC=1.[C:34]1([CH2:40][O:41][C:42]([NH:44][C@H:45]2[CH2:48][NH:47][C:46]2=[O:49])=[O:43])[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1.CN(C1C=CC=CN=1)C>ClCCl>[C:34]1([CH2:40][O:41][C:42]([NH:44][CH:45]2[CH2:48][N:47]([C:46]([N:1]3[CH2:15][CH2:14][CH2:13][C@H:2]3[C:3]([O:5][CH2:6][C:7]3[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=3)=[O:4])=[O:49])[C:23]2=[O:24])=[O:43])[CH:35]=[CH:36][CH:37]=[CH:38][CH:39]=1
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

8

反応物 6

HCID 1140TolueneHCID 6371PhosgeneHCID 8471Triethylamine2 回HCID 218852-DimethylaminopyridineHCID 99767Proline benzyl esterHCID 12834624benzyl N-[(3S)-2-oxoazetidin-3-yl]carbamate

生成物 1

HCID 131714549
(S)-1-[[3-[[(Phenylmethoxy)carbonyl]amino]-2-oxo-1-azetidinyl]carbonyl]-D-proline, phenylmethyl ester

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
-25 °C

実験手順

A solution of d,l-proline, benzyl ester (1.13 grams, 5.5 mmol) in 6 ml of dichloromethane was cooled to 0° C. and 1.2 equivalents (0.92 ml) of triethylamine (668 mg, 6.6 mmol) was added. The resulting mixture was immediately added dropwise to a solution of 20% phosgene in toluene (6 ml, 9.9 mmol) at -25° C. After stirring at -25° C. for 1 hour, the volatiles were evaporated without external heating, and the residue was redissolved in 10 ml of dichloromethane and cooled to 0° C. (S)-3-[[(Phenylmethoxy)carbonyl]amino]-2-azetidinone (1.21 grams, 5.5 mmol) and dimethylaminopyridine (67 mg, 0.55 mmol) were added to the stirring solution. Triethylamine (0.92 ml, 6.6 mmol) was added and the reaction mixture was warmed to room temperature and stirred for 24 hours. The reaction mixture was washed with water, dried over anhydrous Na2SO4, filtered and the dichloromethane removed in vacuo. The residue was purified by flash chromatography on silica gel 230-400 mesh (eluting with 40% ethyl acetate in hexane) yielding 1.2 grams of the title compound as a colorless oil.

後処理

  1. customthe volatiles were evaporated without external heating
  2. dissolutionthe residue was redissolved in 10 ml of dichloromethane
  3. additionwere added to the stirring solution
  4. temperaturethe reaction mixture was warmed to room temperature
  5. stirringstirred for 24 hours
  6. washThe reaction mixture was washed with water
  7. dry with materialdried over anhydrous Na2SO4
  8. filtrationfiltered
  9. customthe dichloromethane removed in vacuo
  10. customThe residue was purified by flash chromatography on silica gel 230-400 mesh (eluting with 40% ethyl acetate in hexane)

出典と根拠

ORDレコード
ord-7d1f728b7dc74347a8ec4713f0ef4163
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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