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Water → HCID 54366438、化合物

HRID 1708332
ノート
印刷プレビュー

反応式

HRID 1708332 の反応式
O=[C:2]1[CH2:21][NH:20][CH:19]2[CH:14]([CH2:15][CH2:16][CH2:17][CH2:18]2)[NH:13][CH2:12][C:11](=O)[NH:10][CH:9]2[CH:4]([CH2:5][CH2:6][CH2:7][CH2:8]2)[NH:3]1.O>O1CCCC1>[CH:9]12[CH2:8][CH2:7][CH2:6][CH2:5][CH:4]1[NH:3][CH2:2][CH2:21][NH:20][CH:19]1[CH:14]([CH2:15][CH2:16][CH2:17][CH2:18]1)[NH:13][CH2:12][CH2:11][NH:10]2
参加物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 962WaterHCID 53848153HCID 53848153、化合物

生成物 1

HCID 54366438HCID 54366438、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A 1M solution of BH3 in tetrahydrofuran (265 ml.) was slowly added to 10.2 g. (33.1 mmol.) of compound (A). The solution was boiled for 24 hours. Water was then added dropwise to destroy the excess BH3 and the reaction mixture was brought to dryness. The solid residue was added to 265 ml. of a 6M hydrochloric acid solution and the mixture was refluxed overnight. Hydrochloric acid was eliminated under vacuum. The residue was digested in ethanol, filtered and dissolved in water. Concentrated ammonia was added until the pH became strongly basic. The inorganic precipitate that formed was filtered off and the filtrate was extracted with methylene chloride yielding 6.3 g. of compound (B) as a white solid after elimination of the solvent.

後処理

  1. customto destroy the excess BH3 and the reaction mixture
  2. additionThe solid residue was added to 265 ml
  3. temperatureof a 6M hydrochloric acid solution and the mixture was refluxed overnight
  4. filtrationfiltered
  5. dissolutiondissolved in water
  6. additionConcentrated ammonia was added until the pH
  7. customThe inorganic precipitate that formed
  8. filtrationwas filtered off
  9. extractionthe filtrate was extracted with methylene chloride yielding 6.3 g

出典と根拠

ORDレコード
ord-4150957ccd5545c98e5601e8f4a7fe41
出典データセット
uspto-grants-1994_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05358704

反応ノート

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