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Acetyl chloride → HCID 10753523、化合物

HRID 2081554
ノート
印刷プレビュー

反応式

HRID 2081554 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:12]([OH:14])=[O:13])[C:5]2[O:10][CH2:9][CH2:8][NH:7][C:6]=2[CH:11]=1.C(N(CC)CC)C.[C:22](Cl)(=[O:24])[CH3:23].C(=O)([O-])O.[Na+]>C(Cl)(Cl)Cl>[C:22]([N:7]1[C:6]2[CH:11]=[C:2]([Cl:1])[CH:3]=[C:4]([C:12]([OH:14])=[O:13])[C:5]=2[O:10][CH2:9][CH2:8]1)(=[O: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

6

反応物 4

HCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 516892Sodium BicarbonateHCID 106086516-Chloro-3,4-dihydro-2H-benzo[b][1,4]oxazine-8-carboxylic acid

生成物 1

HCID 10753523HCID 10753523、化合物収率 65.2%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒
2 回

実験手順

A solution of 10 g of 6-chloro-3,4-dihydro-2H-1,4-benzoxazine-8-carboxylic acid and 6.5 ml of triethylamine in 100 ml of chloroform was cooled, and 4.4 g of acetyl chloride was added thereto with stirring. The resulting mixture was stirred at room temperature for 2 hours. To the liquid reaction mixture were added an aqueous solution of sodium hydrogen carbonate and chloroform, and the resulting organic layer was separated, washed with water, and then dried with magnesium sulfate. The solvent was distilled off under reduced pressure, thereby obtaining 7.8 g of 4-acetyl-6-chloro-3,4-dihydro-2H-1,4-benzoxazine-8-carboxylic acid. Melting point: 76°-77° C.

後処理

  1. stirringThe resulting mixture was stirred at room temperature for 2 hours
  2. customTo the liquid reaction mixture
  3. customthe resulting organic layer was separated
  4. washwashed with water
  5. dry with materialdried with magnesium sulfate
  6. distillationThe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-017b71274f0e4c449f3f5ba9ab26b240
出典データセット
uspto-grants-1993_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05185333

反応ノート

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