Methanol → (1RS,5RS)-4-(4-chlorobenzyl)-1-methyl-6-oxa-bicyclo[3,2,0]heptane-5-carboxyamide

HRID 922743ノート

反応式

HRID 922743 の反応式
ClC1C=CC(CC2[C:13]3([C:14]#[N:15])C(C)(CO3)CC2)=CC=1.COC([C:23]1([CH2:32][C:33]2[CH:38]=[CH:37][C:36]([Cl:39])=[CH:35][CH:34]=2)[CH2:27][CH2:26][C:25]([CH2:29]O)([CH3:28])[C:24]1=[O:31])=O.C[OH:41].[H-].[Na+]>O1CCCC1.O>[Cl:39][C:36]1[CH:35]=[CH:34][C:33]([CH2:32][CH:23]2[C:24]3([CH2:13][C:14]([NH2:15])=[O:41])[C:25]([CH3:28])([CH2:29][O:31]3)[CH2:26][CH2:27]2)=[CH:38][CH:37]=1

参加物

7

反応物 4

HCID 887MethanolHCID 24758Sodium hydrideHCID 672540121-(4-Chlorobenzyl)-3-hydroxymethyl-3-methyl-2-oxocyclopentanecarboxylic acid methyl esterHCID 86718265(1RS,5RS)-4-(4-chlorobenzyl)-1-methyl-6-oxa-bicyclo[3,2,0]heptane-5-carbonitrile

生成物 1

HCID 131734985(1RS,5RS)-4-(4-chlorobenzyl)-1-methyl-6-oxa-bicyclo[3,2,0]heptane-5-carboxyamide

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

In 7 ml of tetrahydrofuran, 703 mg of Compound 5-1 obtained in Production Example 9 of Example 1 was dissolved. To the solution thus obtained, 7 ml of methanol and 5 ml of 25% aqueous solution of sodium hydride were added, and the resulting mixture was refluxed in hot water bath of 80° C. for 5 hours. After the reaction, the solvent was distilled away, and the residue was then mixed with water.

後処理

  1. dissolutionwas dissolved
  2. customTo the solution thus obtained
  3. customAfter the reaction
  4. distillationthe solvent was distilled away
  5. additionthe residue was then mixed with water

出典と根拠

ORDレコード
ord-4a8da9353554476d861acadc75d6fed8
出典データセット
uspto-grants-2016_03
特許番号
US09278966B2

反応ノート

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