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Phenyl chloroformate → phenyl N-[5-[4-[(3S)-3-methylmorpholin-4-yl]-6-(methylsulfonylmethyl)pyrimidin-2-yl]-1,3-thiazol-2-yl]carbamate

HRID 2353697
ノート
印刷プレビュー

反応式

HRID 2353697 の反応式
[CH3:1][C@H:2]1[CH2:7][O:6][CH2:5][CH2:4][N:3]1[C:8]1[CH:13]=[C:12]([CH2:14][S:15]([CH3:18])(=[O:17])=[O:16])[N:11]=[C:10]([C:19]2[S:23][C:22]([NH2:24])=[N:21][CH:20]=2)[N:9]=1.C(=O)([O-])O.[Na+].Cl[C:31]([O:33][C:34]1[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1)=[O:32]>O1CCOCC1>[CH3:1][C@H:2]1[CH2:7][O:6][CH2:5][CH2:4][N:3]1[C:8]1[CH:13]=[C:12]([CH2:14][S:15]([CH3:18])(=[O:17])=[O:16])[N:11]=[C:10]([C:19]2[S:23][C:22]([NH:24][C:31](=[O:32])[O:33][C:34]3[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=3)=[N:21][CH:20]=2)[N:9]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 15891Phenyl chloroformateHCID 516892Sodium BicarbonateHCID 593799205-[4-[(3S)-3-methylmorpholin-4-yl]-6-(methylsulfonylmethyl)pyrimidin-2-yl]-1,3-thiazol-2-amine

生成物 1

HCID 59380033phenyl N-[5-[4-[(3S)-3-methylmorpholin-4-yl]-6-(methylsulfonylmethyl)pyrimidin-2-yl]-1,3-thiazol-2-yl]carbamate

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane
溶媒

実験手順

A solution of 5-[4-[(3S)-3-methylmorpholin-4-yl]-6-(methylsulfonylmethyl)pyrimidin-2-yl]-1,3-thiazol-2-amine (1 g, 2.71 mmol), sodium hydrogen carbonate (342 mg), and phenyl chloroformate (0.511 mL) in dioxane was stirred at RT for 2 hours then concentrated in vacuo. The residue was partitioned between DCM and water and the organic layer dried over sodium sulphate and evaporated to give a foam. The foam was triturated with a mixture of hexane and diethyl ether to give the desired material as a white solid (1.1 g).

後処理

  1. concentrationthen concentrated in vacuo
  2. customThe residue was partitioned between DCM and water
  3. dry with materialthe organic layer dried over sodium sulphate
  4. customevaporated
  5. customto give a foam
  6. customThe foam was triturated with a mixture of hexane and diethyl ether

出典と根拠

ORDレコード
ord-123f072cc6ad400491b8f38a5040c51c
出典データセット
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07750003B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート