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Hydrazine hydrate (1:1) → HCID 11075364、化合物

HRID 1003700
ノート
印刷プレビュー

反応式

HRID 1003700 の反応式
[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([CH2:7][CH2:8][N:9]([CH2:13][CH2:14][CH2:15][CH2:16][N:17]3C(=O)C4=CC=CC=C4C3=O)[CH2:10]2)=[CH:5][CH:4]=1.O.NN>C(O)C>[NH2:17][CH2:16][CH2:15][CH2:14][CH2:13][N:9]1[CH2:8][CH2:7][C:6]2[C:11](=[CH:12][C:3]([O:2][CH3:1])=[CH:4][CH:5]=2)[CH2:10]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 221325287-Methoxy-2-(4-phthalimidobutyl)-1,2,3,4-tetrahydroisoquinoline

生成物 1

HCID 11075364HCID 11075364、化合物収率 63%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 7-methoxy-2-(4-phthalimidobutyl)-1,2,3,4-tetrahydroisoquinoline (17.4 g 0.0478 mol) and hydrazine monohydrate (4.6 ml, 0.095 mol) in ethanol (300 ml) were stirred at room temperature for 18 h and at reflux for 1 h. The cooled reaction mixture was filtered and the filtrate evaporated in vacuo. The residue was dissolved in 2.5N hydrochloric acid, filtered through Kieselguhr and the filtrate basified with 0.880 ammonia. The product was extracted into dichloromethanc (4×200 ml), the combined extracts were dried (Na2SO4) and evaporated in vacuo to afford the title compound as a brown oil (7 g, 63%).

後処理

  1. temperatureat reflux for 1 h
  2. customThe cooled reaction mixture
  3. filtrationwas filtered
  4. customthe filtrate evaporated in vacuo
  5. dissolutionThe residue was dissolved in 2.5N hydrochloric acid
  6. filtrationfiltered through Kieselguhr
  7. extractionThe product was extracted into dichloromethanc (4×200 ml)
  8. dry with materialthe combined extracts were dried (Na2SO4)
  9. customevaporated in vacuo

出典と根拠

ORDレコード
ord-098c271a09bf4d6ca5e79275ec5c86c5
出典データセット
uspto-grants-2000_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06046210

反応ノート

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