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Sulfuric Acid → 2,2,6,6-Tetramethyl-4-hydroxy-4-tert.-butylcarbamoyl piperidine

HRID 1732922
ノート
印刷プレビュー

反応式

HRID 1732922 の反応式
[CH3:1][C:2]1([CH3:13])[CH2:7][C:6]([OH:10])([C:8]#[N:9])[CH2:5][C:4]([CH3:12])([CH3:11])[NH:3]1.[C:14](O)([CH3:17])([CH3:16])[CH3:15].S(=O)(=O)(O)[OH:20]>C(O)(=O)C>[CH3:1][C:2]1([CH3:13])[CH2:7][C:6]([OH:10])([C:8](=[O:20])[NH:9][C:14]([CH3:17])([CH3:16])[CH3:15])[CH2:5][C:4]([CH3:12])([CH3:11])[NH:3]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 6386tert-ButanolHCID 908744-Piperidinecarbonitrile, 4-hydroxy-2,2,6,6-tetramethyl-

生成物 1

HCID 203033412,2,6,6-Tetramethyl-4-hydroxy-4-tert.-butylcarbamoyl piperidine

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

54.6 g 2,2,6,6-Tetramethyl-4-hydroxy-4-cyanopiperidine together with 45 g tert.-butanol in 200 ml glacial acetic acid are introduced into the reactor. Subsequently, 60 g concentrated sulfuric acid are added dropwise with agitation, and agitation is continued for 2 hours at 70° C., thus forming a precipitate which is filtered off and dissolved in water. On alkalization with NaOH, the product precipitates, it is suction-filtered and recrystallized from ethyl acetate. Yield 44 g, m.p. 134°-136° C.

後処理

  1. customthus forming a precipitate which
  2. filtrationis filtered off
  3. dissolutiondissolved in water
  4. customOn alkalization with NaOH, the product precipitates
  5. filtrationit is suction-filtered
  6. customrecrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-deeb7a32d54b48fea464100efeb985de
出典データセット
uspto-grants-1980_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04239891

反応ノート

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