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

HRID 261474노트

반응식

HRID 261474 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-cbc26c2cf760444590ea819f9863aaa2
출처 데이터셋
uspto-grants-1979_08
특허 번호
US04166120

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