Water → 4-(3'-Azidopropyl)-piperidine

HRID 903863

反応式

HRID 903863 の反応式
[N-:1]=[N+:2]=[N-:3].[Na+].Br.Br[CH2:7][CH2:8][CH2:9][CH:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1.O>CO>[N:1]([CH2:7][CH2:8][CH2:9][CH:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1)=[N+:2]=[N-:3]

参加物

5

反応物 3

HCID 962WaterHCID 33557Sodium AzideHCID 135032154-(3-Bromopropyl)piperidine hydrobromide

生成物 1

HCID 135032204-(3'-Azidopropyl)-piperidine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Sodium azide (1 g) was added to a mixture of 4-(3'-bromopropyl)-piperidine hydrobromide (2 g), water (7 ml) and methanol (7 ml). The pH of the mixture was adjusted to 6.3, and the resulting solution was refluxed for 2 hours. After cooling, methanol was evaporated, 30 percent aqueous sodium hydroxide was added and the mixture was extracted several times with ether. The ether extracts were dried and evaporated to leave the desired compound as an oil. The IR-spectrum (CHCl3) showed strong bands at 2925, 2100 and 1450 cm-1.

後処理

  1. temperaturethe resulting solution was refluxed for 2 hours
  2. temperatureAfter cooling
  3. custommethanol was evaporated
  4. addition30 percent aqueous sodium hydroxide was added
  5. extractionthe mixture was extracted several times with ether
  6. dry with materialThe ether extracts were dried
  7. customevaporated

出典と根拠

ORDレコード
ord-806b04d0240c4ed3bee89453fef8cddb
出典データセット
uspto-grants-1980_10
特許番号
US04229443

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