Lithium hydroxide, monohydrate → HCID 15864131, 화합물

HRID 842256노트

반응식

HRID 842256 반응식
C([O:4][CH2:5][CH2:6][C:7]([NH:33]C(=O)C)([CH2:28][O:29]C(=O)C)[CH2:8][CH2:9][CH2:10][C:11]1[CH:16]=[CH:15][C:14]([CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27])=[CH:13][CH:12]=1)(=O)C.O.[OH-].[Li+]>CO.O>[NH2:33][C:7]([CH2:8][CH2:9][CH2:10][C:11]1[CH:16]=[CH:15][C:14]([CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27])=[CH:13][CH:12]=1)([CH2:6][CH2:5][OH:4])[CH2:28][OH:29]

참가 물질

5

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 15864135HCID 15864135, 화합물

생성물 1

HCID 15864131HCID 15864131, 화합물수율 25.9%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매2회

실험 절차

3-Acetamido-3-acetoxymethyl-6-(4-undecylphenyl)hexyl acetate (1.70 g) and lithium hydroxide monohydrate (1.42 g) were dissolved in methanol (17 ml) and water (17 ml), and the mixture was refluxed under heating for 3 hours while stirring. The reaction mixture was diluted with water (100 ml) and extracted with ethyl acetate. The ethyl acetate layer was dried over anhydrous sodium sulfate and the solvent was distilled away. The crude crystals obtained were recrystallized from ether-hexane-ethyl acetate (2:2:1) to give the subject compound (330 mg) as white crystals, melting at 73-76° C.

후처리

  1. temperatureunder heating for 3 hours
  2. extractionextracted with ethyl acetate
  3. dry with materialThe ethyl acetate layer was dried over anhydrous sodium sulfate
  4. distillationthe solvent was distilled away
  5. customThe crude crystals obtained
  6. customwere recrystallized from ether-hexane-ethyl acetate (2:2:1)

출처 및 근거

ORD 기록
ord-eab21fc41cf1420ab3a0f5af3b647dbf
출처 데이터셋
uspto-grants-2002_04
특허 번호
US06372800B1

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