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2-Aminophenol → 2-(3-bromopropyl)-2H-1,4-benzoxazine-3(4H)-one

HRID 2259572
ノート
印刷プレビュー

反応式

HRID 2259572 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[OH:8].Br[CH:10]([CH2:15][CH2:16][CH2:17][Br:18])[C:11](OC)=[O:12].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O.C(OCC)C>[Br:18][CH2:17][CH2:16][CH2:15][CH:10]1[C:11](=[O:12])[NH:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=2[O:8]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 58012-AminophenolHCID 11430Potassium CarbonateHCID 10912698Methyl 2,5-dibromopentanoate

生成物 1

HCID 143046582-(3-bromopropyl)-2H-1,4-benzoxazine-3(4H)-one収率 20.3%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 3283Diethyl Ether溶媒

実験手順

24 g of 2-aminophenol, 55 g of methyl 2,5-dibromovalerate and 30 g of potassium carbonate were heated to reflux for 5 hours in 250 ml of acetone. For work-up, the reaction mixture was diluted with 250 ml of diethyl ether, washed with 200 ml of water and acidified to pH=1 using 12N hydrochloric acid solution. The organic phase was separated, washed twice with 100 ml of water each time, dried and evaporated. The residue was crystallized from methanol. 11 g of 2-(3-bromopropyl)-2H-1,4-benzoxazin-3(4H)one were obtained.

後処理

  1. washwashed with 200 ml of water
  2. customThe organic phase was separated
  3. washwashed twice with 100 ml of water each time
  4. customdried
  5. customevaporated
  6. customThe residue was crystallized from methanol

出典と根拠

ORDレコード
ord-2becd2a960734871baacef005f50af07
出典データセット
uspto-grants-1995_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05474988

反応ノート

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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