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Sodium Hydroxide → HCID 54179458、化合物

HRID 372560
ノート
印刷プレビュー

反応式

HRID 372560 の反応式
[OH-].[Na+].Cl.[Cl:4][C:5]1[CH:18]=[CH:17][C:8]2[CH2:9][CH2:10][CH:11]([NH:15][CH3:16])[CH2:12][C:13](=[O:14])[C:7]=2[CH:6]=1>O>[Cl:4][C:5]1[CH:18]=[CH:17][C:8]2[CH2:9][CH2:10][CH:11]([NH:15][CH3:16])[CH2:12][CH:13]([OH:14])[C:7]=2[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

4

反応物 2

HCID 14798Sodium HydroxideHCID 131711106HCID 131711106、化合物

生成物 1

HCID 54179458HCID 54179458、化合物収率 92.7%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
10 °C

実験手順

Sodium hydroxide solution was added to suspension of 4.6 g of the product of Step B in 100 ml of water cooled to 10° C and the mixture was extracted with methylene chloride. The extracts were dried and evaporated to dryness and the 4 g of oily residue were dissolved in 40 ml of ethanol and 4 ml of water. 2 g of sodium borohydride were added to the mixture at 20° C and the mixture was stirred for an hour. The mixture was evaporated to dryness and the residue was taken up in methylene chloride. The solution was washed with water, dried and evaporated to dryness. The residue was washed with isopropyl ether to obtain 3.7 g of 3-chloro-5ξ-hydroxy-7-methylamino-6,7,8,9-tetrahydro [5H] benzocycloheptene melting at 90° C.

後処理

  1. extractionthe mixture was extracted with methylene chloride
  2. customThe extracts were dried
  3. customevaporated to dryness
  4. dissolutionthe 4 g of oily residue were dissolved in 40 ml of ethanol
  5. addition2 g of sodium borohydride were added to the mixture at 20° C
  6. customThe mixture was evaporated to dryness
  7. washThe solution was washed with water
  8. customdried
  9. customevaporated to dryness
  10. washThe residue was washed with isopropyl ether

出典と根拠

ORDレコード
ord-6088029bf0b246da8b337fcd30ae95d3
出典データセット
uspto-grants-1978_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04091115

反応ノート

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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