ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Hydrochloric Acid → Ethanol, 2-((1-(3-(10H-phenothiazin-10-yl)propyl)-4-piperidinyl)oxy)-, monohydrochloride

HRID 329036
ノート
印刷プレビュー

反応式

HRID 329036 の反応式
[I-].[Na+].[Cl:3][CH2:4][CH2:5][CH2:6][N:7]1[C:20]2[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=2[S:14][C:13]2[C:8]1=[CH:9][CH:10]=[CH:11][CH:12]=2.C(N(CC)CC)C.[NH:28]1[CH2:33][CH2:32][CH:31]([O:34][CH2:35][CH2:36][OH:37])[CH2:30][CH2:29]1.Cl>C(C(C)=O)C.CCOCC>[ClH:3].[OH:37][CH2:36][CH2:35][O:34][CH:31]1[CH2:32][CH2:33][N:28]([CH2:4][CH2:5][CH2:6][N:7]2[C:20]3[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=3[S:14][C:13]3[C:8]2=[CH:9][CH:10]=[CH:11][CH:12]=3)[CH2:29][CH2:30]1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 5238Sodium IodideHCID 8471TriethylamineHCID 1229912010-(3-chloropropyl)-10H-phenothiazineHCID 202953322-(Piperidin-4-yloxy)ethan-1-ol

生成物 1

HCID 218308Ethanol, 2-((1-(3-(10H-phenothiazin-10-yl)propyl)-4-piperidinyl)oxy)-, monohydrochloride収率 55.4%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒2 回HCID 6569Methyl Ethyl Ketone溶媒

実験手順

22.5 g (0.15 mole) of sodium iodide was added to a solution of 41.5 g (0.15 mole) of 10-(3-chloropropyl)-phenothiazine in 400 ml of methyl ethyl ketone and then 15.2 g (0.15 mole) of triethylamine followed by 21.7 g (0.15 mole) of 2-(4-piperidyloxy)-ethanol were added to the reaction mixture. The solution was refluxed with stirring for 20 hours and after cooling, the precipitate formed was removed by vacuum filtration. The filtrate was evaporated to dryness and the oily residue was extracted with aqueous hydrochloric acid. The acidic extract was washed with ether, made alkaline and was extracted with benzene. The benzene phase was repeatedly washed with water, dried and concentrated to obtain an oil. The oil was dissolved in ether and hydrogen chloride in ether was added thereto. The precipitate was recoved by vacuum filtration and was crystallized from a 95% ethanol-ether mixture to obtain 35 g (55% yield) of 10-[3-(4-β-hydroxyethoxypiperidino)-propyl]-phenothiazine hydrochloride in the form of white crystals melting at 183° C on a heated microscopic stage. The product was identical to that of Example XI.

後処理

  1. additionwere added to the reaction mixture
  2. temperatureThe solution was refluxed
  3. temperatureafter cooling
  4. customthe precipitate formed
  5. customwas removed by vacuum filtration
  6. customThe filtrate was evaporated to dryness
  7. extractionthe oily residue was extracted with aqueous hydrochloric acid
  8. extractionThe acidic extract
  9. washwas washed with ether
  10. extractionwas extracted with benzene
  11. washThe benzene phase was repeatedly washed with water
  12. customdried
  13. concentrationconcentrated
  14. customto obtain an oil
  15. filtrationThe precipitate was recoved by vacuum filtration
  16. customwas crystallized from a 95% ethanol-ether mixture

出典と根拠

ORDレコード
ord-f0f9e570c2f94fb292e7991327982bb8
出典データセット
uspto-grants-1977_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04018922

反応ノート

読み込み中…

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