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Phosgene → 6-[4-(Benzenesulfinyl)butoxy]-1,4-dihydro-2H-3,1-benzoxazin-2-one

HRID 463217
ノート
印刷プレビュー

反応式

HRID 463217 の反応式
[NH2:1][C:2]1[CH:9]=[CH:8][C:7]([O:10][CH2:11][CH2:12][CH2:13][CH2:14][S:15]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[O:16])=[CH:6][C:3]=1[CH2:4][OH:5].[C:23](=O)([O-])[O-:24].[K+].[K+].C(Cl)(Cl)=O>C(Cl)(Cl)Cl.C1(C)C=CC=CC=1>[C:17]1([S:15]([CH2:14][CH2:13][CH2:12][CH2:11][O:10][C:7]2[CH:8]=[CH:9][C:2]3[NH:1][C:23](=[O:24])[O:5][CH2:4][C:3]=3[CH:6]=2)=[O:16])[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 6371PhosgeneHCID 11430Potassium CarbonateHCID 566193032-Amino-5-(4-phenylsulfinylbutoxy)-benzyl alcohol

生成物 1

HCID 132605746-[4-(Benzenesulfinyl)butoxy]-1,4-dihydro-2H-3,1-benzoxazin-2-one

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 6212Chloroform溶媒

実験手順

An amount of 4.2 gm (0.0133 mol) of 2-amino-5-(4-phenylsulfinylbutoxy)-benzyl alcohol [prepared from 2-nitro-5-(4-phenylsulfinyl-butoxy)-benzyl alcohol by catalytic hydrogenation] is dissolved in 150 ml of chloroform and mixed with 6.9 gm (0.05 mol) of potassium carbonate. Ten milliliters of a 20% solution of phosgene in toluene is slowly added dropwise to this mixture under stirring. After further stirring for two hours, the solution is washed with water and dried with sodium sulfate, and the solvents are distilled off in vacuo. The residue is recrystallized from ethyl acetate/cyclohexane.

後処理

  1. stirringAfter further stirring for two hours
  2. washthe solution is washed with water
  3. dry with materialdried with sodium sulfate
  4. distillationthe solvents are distilled off in vacuo
  5. customThe residue is recrystallized from ethyl acetate/cyclohexane

出典と根拠

ORDレコード
ord-f272e97895fb498895b36de5ac28fbe3
出典データセット
uspto-grants-1985_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04518597

反応ノート

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