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Sodium borohydride → Sodium Hydroxide

HRID 842078
ノート
印刷プレビュー

反応式

HRID 842078 の反応式
[CH3:1][N:2]1[C@@H:12]2[CH2:13][C:14]3[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[C:16]([OH:22])[C:15]=3[C@@:5]3([C:11]2=[CH:10][C:8](=[O:9])[C:7]([O:23][CH3:24])=[CH:6]3)[CH2:4][CH2:3]1.CN1[C@@H]2CC3C=CC(OC)=C4O[C@H]5C(OC)=CC=C2[C@]5(C=34)CC1.C1C2C[C@H]3N(CC[C@@]45[C@H]3C=C[C@H](O)[C@@H]4OC(C=25)=C(O)C=1)C.CN1[C@H]2CC3C=CC(OC)=C(O)C=3[C@]3([C@@H]2C=C(OC)C(=O)C3)CC1.NC1C(OCC2C=CC=CC=2)=C(OC)C=CC=1CC1C2C(=CC(OC)=C(OC)C=2)CCN1C.[BH4-].[Na+:127]>CO>[CH3:1][N:2]1[C@@H:12]2[CH2:13][C:14]3[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[C:16]4[O:22][C@H:6]5[C:7]([O:23][CH3:24])=[CH:8][CH:10]=[C:11]2[C@:5]5([C:15]=34)[CH2:4][CH2:3]1.[OH-:9].[Na+:127]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 6

HCID 4311764Sodium borohydrideHCID 5288826MorphineHCID 5324289Thebaine2 回HCID 5408233Salutaridine3 回HCID 5459308SinomenineHCID 22289810(+/-) 1-(2-Amino-3-benzyloxy-4-methoxybenzyl)-1,2,3,4,-tetrahydro-6,7-dimethoxy-2-methylisoquinoline

生成物

2
HCID 14798Sodium Hydroxide収率 10%HCID 5324289Thebaine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

N-demethyl-sinomenine may be also be obtained through total synthesis, e.g. by adaptation of the procedures described by Kametani et al., (Kametani, T., et al., Studies on the synthesis of heterocyclic compounds. Part ccc. Synthesis of salutridine, sinoacutine, and thebaine. Formal total syntheses of morphine and sinomenine., J. Chem. Soc. (C), 15:2030-2033 (1969)). Specifically, total synthesis begins with diazotization of (±) 1-(2-amino-3-benzyloxy-4-methoxybenzyl)-1,2,3,4,-tetrahydro-6,7-dimethoxy-2-methylisoquinoline, followed by the thermal decomposition of the resulting diazonium salt. The result would be (±) salutaridine which is converted into (±) thebaine by incubation of (±) salutaridine with methanol and sodium borohydride. After incubation at 0° C. for 1 hour, evaporation of methanol, and extraction with 10% aqueous ammonium chloride and chloroform, the resulting intermediate, a mixture of epimeric alcohols, is treated with N-hydrochloric acid for 1 hour. From this solution (±) thebaine is isolated by liquid-liquid extraction (addition of 10% sodium hydroxide and extraction into chloroform) and a solid liquid purification step using preparative thick-layer chromatography on a silica gel. (±) N-demethyl sinomenine is then synthesized from (±) thebaine using a modification of the procedure of Okabe K., et al., Jap. J. Pharm. Chem. 39:267 (1968). As an alternative to total synthesis, the intermediate products (±) salutaridine or (±) thebaine could be used as starters for N-demethyl-sinomenine synthesis.

後処理

  1. customSpecifically, total synthesis
  2. customThe result would
  3. customevaporation of methanol, and extraction with 10% aqueous ammonium chloride and chloroform
  4. additionthe resulting intermediate, a mixture of epimeric alcohols
  5. additionis treated with N-hydrochloric acid for 1 hour

出典と根拠

ORDレコード
ord-3d877158479847d4b95083616c065cb6
出典データセット
uspto-grants-2002_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06372756B1

反応ノート

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