Acetyl chloride → 2,3-Dihydro-1'-acetylspiro[benzofuran-2,4'-piperidine]

HRID 261474ノート

反応式

HRID 261474 の反応式
[C:1](Cl)(=[O:3])[CH3:2].[NH:5]1[CH2:10][CH2:9][C:8]2([CH2:14][C:13]3[CH:15]=[CH:16][CH:17]=[CH:18][C:12]=3[O:11]2)[CH2:7][CH2:6]1.C(=O)(O)[O-].[Na+]>C(Cl)(Cl)Cl>[C:1]([N:5]1[CH2:10][CH2:9][C:8]2([CH2:14][C:13]3[CH:15]=[CH:16][CH:17]=[CH:18][C:12]=3[O:11]2)[CH2:7][CH2:6]1)(=[O:3])[CH3:2]

参加物

5

反応物 3

HCID 6367Acetyl chlorideHCID 516892Sodium BicarbonateHCID 127332303H-Spiro(1-benzofuran-2,4'-piperidine)

生成物 1

HCID 127332342,3-Dihydro-1'-acetylspiro[benzofuran-2,4'-piperidine]

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

3 ml of acetyl chloride in 10 ml of chloroform is added dropwise to a stirred suspension of 6.0 g of 2,3-dihydrospiro[benzofuran-2,4'-piperidine], Example 1C, and 14.0 g of sodium bicarbonate in 75 ml of chloroform. After total addition, the reaction mixture is successively stirred at ambient temperature for 16 hours, filtered, washed sequentially with water, dilute hydrochloric acid and a saturated sodium chloride solution, dried and the solvent removed under reduced pressure, leaving a residue which solidifies upon standing. The solid is recrystallized twice from hexane to give the product, 2,3-dihydro-1'-acetylspiro[benzofuran-2,4'-piperidine], mp 94°-97° C.

後処理

  1. additionAfter total addition
  2. filtrationfiltered
  3. washwashed sequentially with water, dilute hydrochloric acid
  4. dry with materiala saturated sodium chloride solution, dried
  5. customthe solvent removed under reduced pressure
  6. customleaving a residue which
  7. customThe solid is recrystallized twice from hexane

出典と根拠

ORDレコード
ord-cbc26c2cf760444590ea819f9863aaa2
出典データセット
uspto-grants-1979_08
特許番号
US04166120

反応ノート

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