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Dichloromethane → HCID 20452304、化合物

HRID 1462976
ノート
印刷プレビュー

反応式

HRID 1462976 の反応式
O[C:2]1[CH:11]=[C:10]2[C:5]([CH2:6][CH2:7][NH:8][CH:9]2[CH2:12][C:13]2[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[C:15]([OH:21])[CH:14]=2)=[CH:4][C:3]=1[O:22][CH3:23].[C:24](=[O:27])(O)[O-].[Na+].[CH2:29](Br)[CH:30]=[CH2:31].F[C:34](F)(F)C(O)=O.C(Cl)[Cl:41]>O=[V].Cl.Cl.Cl.C(O)C>[ClH:41].[CH2:29]([N:8]1[CH:9]2[C:10]3=[C:11]([C:2]([O:27][CH3:24])=[C:3]([O:22][CH3:23])[CH:4]=[C:5]3[CH2:6][CH2:7]1)[C:18]1[CH:17]=[C:16]([O:19][CH3:20])[C:15]([O:21][CH3:34])=[CH:14][C:13]=1[CH2:12]2)[CH:30]=[CH2:31]
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 6344Dichloromethane2 回HCID 6422Trifluoroacetic acidHCID 7841Allyl bromideHCID 443766(+-)-NorreticulineHCID 516892Sodium Bicarbonate

生成物 1

HCID 20452304HCID 20452304、化合物

試薬・触媒・溶媒 2

HCID 24410
Vanadium trichloride oxide
触媒
HCID 702Ethanol溶媒

実験手順

8.0 g. (25.37 mmol) (+)-7-Hydroxy-1-(3-hydroxy-4-methoxybenzyl)-6-methoxy-1,2,3,4-tetrahydroisoquinoline (J. Org. Chem., 45, 592/1980) in 150 ml. ethanol are mixed with 5.10 g. (60.7 mmol) sodium bicarbonate and 2.19 ml. (3.07 g.) allyl bromide in a manner analogous to that described in Example 1. The N-allylation product (8.0 g., 22.5 mmol, yellowish foam) obtained after appropriate working up is reacted at -10° C. in a mixture of 70 ml. trifluoroacetic acid and 70 ml. methylene chloride with 3.2 ml. (5.89 g., 33.98 mmol) vanadium oxytrichloride in 35 ml. anhydrous methylene chloride in a manner analogous to that described in Example 1. The crude product obtained (8 g., crystallisation from chloroform/diethyl ether; m.p. 159°-165° C.) is O-methylated in a manner analogous to that described in Example 1 with 115 ml. of a 1N solution of phenyltrimethylammonium hydroxide in methanol in 400 ml. of a mixture of toluene and dimethylformamide (9:1 v/v). The crude product obtained after appropriate working up is, after chromatographic purification on silica gel with chloroform as elution agent, converted with ethanolic hydrochloric acid into the crystalline hydrochloride. There is obtained (-)-6-allyl-5,6,6a,7-tetrahydro-1,2,9,10-tetramethoxy-4H-dibenzo(de,g)quinoline hydrochloride; m.p. 210°-217° C.

後処理

  1. customThe N-allylation product (8.0 g., 22.5 mmol, yellowish foam) obtained
  2. customafter appropriate working up is reacted at -10° C. in a mixture of 70 ml
  3. customThe crude product obtained
  4. custom(8 g., crystallisation from chloroform/diethyl ether; m.p. 159°-165° C.)
  5. additionof a mixture of toluene and dimethylformamide (9:1 v/v)
  6. customThe crude product obtained
  7. customafter chromatographic purification on silica gel with chloroform
  8. washas elution agent

出典と根拠

ORDレコード
ord-d9ed27e345c14a6eb7cc38bc0d8700cd
出典データセット
uspto-grants-1984_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04461895

反応ノート

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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