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Hydrogen Peroxide → 1-Phenyl-8-[(cis-1,2,3,4-tetrahydro-1-hydroxy-2-naphthalenyl)methyl]-1,3,8-triazaspiro[4.5]decan-4-one

HRID 2072459
ノート
印刷プレビュー

反応式

HRID 2072459 の反応式
[C:1]1([N:7]2[C:11]3([CH2:16][CH2:15][N:14]([CH2:17][CH:18]4[CH2:27][CH2:26][C:25]5[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=5)[C:19]4=[O:28])[CH2:13][CH2:12]3)[C:10](=[O:29])[NH:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C([BH-](C(CC)C)C(CC)C)(CC)C.[Li+].[OH-].[Na+].OO.C(=O)([O-])[O-].[K+].[K+]>O1CCCC1>[C:1]1([N:7]2[C:11]3([CH2:16][CH2:15][N:14]([CH2:17][C@H:18]4[CH2:27][CH2:26][C:25]5[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=5)[C@H:19]4[OH:28])[CH2:13][CH2:12]3)[C:10](=[O:29])[NH:9][CH2:8]2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 784Hydrogen PeroxideHCID 11430Potassium CarbonateHCID 14798Sodium HydroxideHCID 3611392Lithium tri-s-butylborohydrideHCID 214082211-Phenyl-8-[(1,2,3,4-tetrahydro-1-oxo-2-naphthalenyl)methyl]-1,3,8-triazaspiro[4.5]decan-4-one

生成物 1

HCID 54521082
1-Phenyl-8-[(cis-1,2,3,4-tetrahydro-1-hydroxy-2-naphthalenyl)methyl]-1,3,8-triazaspiro[4.5]decan-4-one

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
-78 °C

実験手順

1-Phenyl-8-[(1,2,3,4-tetrahydro-1-oxo-2-naphthalenyl)methyl]-1,3,8-triazaspiro[4.5]decan-4-one (5.0 g) is dissolved in 60 ml of dry tetrahydrofuran and added, dropwise, to a flask charged with 2.1 equivalents of a 1 molar tetrahydrofuran solution of lithium tri-sec-butylborohydride, previously cooled to -78° C, all under an argon atmosphere. The resulting solution is stirred for 16 hours at room temperature. The reaction mixture is treated at 0° C with 15 ml of 3 molar sodium hydroxide followed by the addition of 15 ml of 30% hydrogen peroxide. The aqueous phase is saturated with potassium carbonate and the organic layer is separated and concentrated. The residue is dissolved in methylene chloride, washed with water, dried and concentrated producing the crude product. Recrystallization of this material from methylene chloride/hexane yields 4.2 g of isomerically pure title compound, melting point 204°-205° C.

後処理

  1. additionadded
  2. customthe organic layer is separated
  3. concentrationconcentrated
  4. dissolutionThe residue is dissolved in methylene chloride
  5. washwashed with water
  6. customdried
  7. concentrationconcentrated
  8. customproducing the crude product
  9. customRecrystallization of this material from methylene chloride/hexane

出典と根拠

ORDレコード
ord-8fdc1bfa7b794789be38be12786ac19a
出典データセット
uspto-grants-1977_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04051248

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート