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Formaldehyde → HCID 13755079、化合物

HRID 2309191
ノート
印刷プレビュー

反応式

HRID 2309191 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([CH:13]2[CH2:18][CH2:17][CH2:16][NH:15][CH2:14]2)=[C:7]2[C:11]=1[NH:10][C:9](=[O:12])[CH2:8]2.[CH2:19]=O.[BH4-].[Na+]>CO.O>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([CH:13]2[CH2:18][CH2:17][CH2:16][N:15]([CH3:19])[CH2:14]2)=[C:7]2[C:11]=1[NH:10][C:9](=[O:12])[CH2:8]2
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

6

反応物 3

HCID 712FormaldehydeHCID 4311764Sodium borohydrideHCID 13755077HCID 13755077、化合物

生成物 1

HCID 13755079HCID 13755079、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

反応条件

温度
5 °C

実験手順

4.5 g of the product of Example 1 were dissolved in 100 ml of methanol with stirring under an inert atmosphere and after cooling to about 5° C., 3.4 ml of 40% formic aldehyde were added dropwise. After stirring for 1 hour, 1.8 g of 95% sodium borohydride were added in small fractions and the mixture was stirred for 1 hour. The temperature was allowed to return to ambient and after diluting with iced water, extracting with methylene chloride, drying and evaporating to dryness under reduced pressure, filtering, washing with ether and drying, 4 g of 1,3-dihydro-7-methoxy-4-(1-methyl-3-piperidinyl)-2H-indol-2-one were obtained in the form of a base melting at ≃170° C.

後処理

  1. stirringAfter stirring for 1 hour
  2. stirringthe mixture was stirred for 1 hour
  3. extractionextracting with methylene chloride
  4. customdrying
  5. customevaporating to dryness under reduced pressure
  6. filtrationfiltering
  7. washwashing with ether
  8. customdrying

出典と根拠

ORDレコード
ord-af3574abc65b4b5cae45c2d7b6f2f9cc
出典データセット
uspto-grants-1987_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04694011

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