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

HRID 918234노트

반응식

HRID 918234 반응식
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

참가 물질

5

반응물 2

HCID 223976024-Piperidinone, 2,2,6,6-tetramethyl-, monohydrateHCID 178511210HCID 178511210, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 8471Triethylamine촉매HCID 3776Isopropanol용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-a7a8c00de87c44faa87768b4ab2ec999
출처 데이터셋
uspto-grants-1976_07
특허 번호
US03970636

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