1-Butanol → HCID 20338287, 화합물

HRID 1395806노트

반응식

HRID 1395806 반응식
Cl.[CH2:2]([N:9]([CH2:19][CH2:20][Cl:21])[C:10]1[CH:18]=[CH:17][CH:16]=[CH:15][C:11]=1[C:12]([NH2:14])=[O:13])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.C([O-])([O-])=O.[Na+].[Na+].[OH:28][C:29]1([C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)[CH2:34][CH2:33][NH:32][CH2:31][CH2:30]1.C(O)CCC>C(Cl)(Cl)Cl>[ClH:21].[CH2:2]([N:9]([CH2:19][CH2:20][N:32]1[CH2:33][CH2:34][C:29]([OH:28])([C:35]2[CH:36]=[CH:37][CH:38]=[CH:39][CH:40]=2)[CH2:30][CH2:31]1)[C:10]1[CH:18]=[CH:17][CH:16]=[CH:15][C:11]=1[C:12]([NH2:14])=[O:13])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1

참가 물질

6

반응물 4

HCID 2631-ButanolHCID 10340Sodium CarbonateHCID 963874-Phenylpiperidin-4-olHCID 20338242HCID 20338242, 화합물

생성물 1

HCID 20338287HCID 20338287, 화합물수율 53.8%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

A mixture of 19.5 g 2-[Benzyl(2-chloroethyl)amino]benzamide hydrochloride, 15.75 g powdered anhydrous Na2CO3, 10.6 g 4-hydroxy-4-phenylpiperidine and 250 ml butanol was refluxed 20 hours, cooled and an equal volume of chloroform added. The mixture was filtered and the filtrate concentrated on the rotovap to dryness. The residue was dissolved in 500 ml ether, a little dry ice added, the mixture filtered and concentrated to dryness. The residue in 300 ml ether was treated with dry HC1 and filtered to give 15 g product.

후처리

  1. temperaturewas refluxed 20 hours
  2. temperaturecooled
  3. filtrationThe mixture was filtered
  4. concentrationthe filtrate concentrated on the rotovap to dryness
  5. dissolutionThe residue was dissolved in 500 ml ether
  6. additiona little dry ice added
  7. filtrationthe mixture filtered
  8. concentrationconcentrated to dryness
  9. additionThe residue in 300 ml ether was treated with dry HC1
  10. filtrationfiltered

출처 및 근거

ORD 기록
ord-1de9394dd11f4aceb7150afe9d9682c8
출처 데이터셋
uspto-grants-1980_05
특허 번호
US04205173

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