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Sodium Bicarbonate → HCID 18957084、化合物

HRID 2379590
ノート
印刷プレビュー

反応式

HRID 2379590 の反応式
F[B-](F)(F)F.C([O+:8]([CH2:11][CH3:12])[CH2:9][CH3:10])C.[Cl:13][C:14]1[CH:22]=C2[C:17]([CH2:18][NH:19]C2=O)=[CH:16][CH:15]=1.C(=O)([O-])O.[Na+]>C(Cl)Cl>[CH2:11]([O:8][C:9]1[C:10]2[C:17](=[CH:16][CH:15]=[C:14]([Cl:13])[CH:22]=2)[CH2:18][N:19]=1)[CH3:12]
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 516892Sodium BicarbonateHCID 2723982Triethyloxonium tetrafluoroborateHCID 124964756-Chloro-2,3-dihydro-1H-isoindol-1-one

生成物 1

HCID 18957084HCID 18957084、化合物収率 88.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 151 g of triethyloxonium tetrafluoroborate in 3,200 ml of methylene chloride was stirred under argon at room temperature for 3.5 hours after the addition of 106.6 g of 6-chloro-2, 3-dihydro-1H-isoindol-1-one. The mixture was then treated within 40 minutes with 1.28 l of saturated sodium hydrogen carbonate solution, the organic phase was separated and washed with 1.28 l of water. After drying over sodium sulphate the organic phase was filtered and evaporated. The residue was taken up in 1.3 l of diethyl ether, whereupon it was stirred at room temperature for about 30 minutes. After removing insoluble material by filtration the filtrate was evaporated. There was obtained 110.5 g of 1-ethoxy-6-chloro-3H-isoindole with a m.p. of 64°-66°.

後処理

  1. customthe organic phase was separated
  2. washwashed with 1.28 l of water
  3. dry with materialAfter drying over sodium sulphate the organic phase
  4. filtrationwas filtered
  5. customevaporated
  6. customAfter removing insoluble material
  7. filtrationby filtration the filtrate
  8. customwas evaporated

出典と根拠

ORDレコード
ord-84c631f1740942079f1b37660aa047d8
出典データセット
uspto-grants-1994_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05362738

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