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Acetyl chloride → HCID 10753523, 화합물

HRID 2081554
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HRID 2081554 반응식
[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]
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참가 물질

6

반응물 4

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

생성물 1

HCID 10753523HCID 10753523, 화합물수율 65.2%

시약·촉매·용매 1

HCID 6212Chloroform
용매
2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-017b71274f0e4c449f3f5ba9ab26b240
출처 데이터셋
uspto-grants-1993_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05185333

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