4-Piperidinone, 2,2,6,6-tetramethyl-, monohydrate → (2,2,6,6-Tetramethyl-4-hydroxy-4-piperidinyl)bis(2-cyanoethyl)phosphine oxide

HRID 918234

反応式

HRID 918234 の反応式
O.[CH3:2][C:3]1([CH3:12])[CH2:8][C:7](=[O:9])[CH2:6][C:5]([CH3:11])([CH3:10])[NH:4]1.[C:13]([CH2:15][CH2:16][PH:17](=[O:22])[CH2:18][CH2:19][C:20]#[N:21])#[N:14]>C(N(CC)CC)C.C(O)(C)C>[CH3:2][C:3]1([CH3:12])[CH2:8][C:7]([P:17](=[O:22])([CH2:18][CH2:19][C:20]#[N:21])[CH2:16][CH2:15][C:13]#[N:14])([OH:9])[CH2:6][C:5]([CH3:11])([CH3:10])[NH:4]1

参加物

5

反応物 2

HCID 223976024-Piperidinone, 2,2,6,6-tetramethyl-, monohydrateHCID 178511210HCID 178511210、化合物

生成物 1

HCID 21521477(2,2,6,6-Tetramethyl-4-hydroxy-4-piperidinyl)bis(2-cyanoethyl)phosphine oxide収率 65%

試薬・触媒・溶媒 2

HCID 8471Triethylamine触媒HCID 3776Isopropanol溶媒

実験手順

To 100 milliliters of isopropanol was added 8.65 grams (0.05 mole) of 2,2,6,6-tetramethyl-4-piperidone hydrate; 7.81 grams (0.05 mole) of bis(2-cyanoethyl)phosphine oxide; and 1 gram of triethylamine as catalyst. The reaction mixture was refluxed four hours, cooled in an ice bath, and the crystalline product filtered off. After recrystallization, there was obtained 10.0 grams of white crystalline product of 128°-130°C. melting point, representing a 65% yield.

後処理

  1. temperatureThe reaction mixture was refluxed four hours
  2. temperaturecooled in an ice bath
  3. filtrationthe crystalline product filtered off
  4. customAfter recrystallization

出典と根拠

ORDレコード
ord-a7a8c00de87c44faa87768b4ab2ec999
出典データセット
uspto-grants-1976_07
特許番号
US03970636

関連ノート

読み込み中…