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Diazomethane → Methyl 7-[2-(3-Hydroxy-4-propoxybutyl)-1,4-dioxo-3-thiazolidinyl]heptanoate

HRID 867120
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HRID 867120 반응식
[N+](=[CH2:3])=[N-].[OH:4][CH:5]([CH2:24][O:25][CH2:26][CH2:27][CH3:28])[CH2:6][CH2:7][CH:8]1[N:12]([CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][C:19]([OH:21])=[O:20])[C:11](=[O:22])[CH2:10][S:9]1=[O:23]>CCOCC>[OH:4][CH:5]([CH2:24][O:25][CH2:26][CH2:27][CH3:28])[CH2:6][CH2:7][CH:8]1[N:12]([CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][C:19]([O:21][CH3:3])=[O:20])[C:11](=[O:22])[CH2:10][S:9]1=[O:23]
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참가 물질

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반응물 2

HCID 9550DiazomethaneHCID 203173927-[2-(3-Hydroxy-4-propoxybutyl)-1,4-dioxo-3-thiazolidinyl]heptanoic Acid

생성물 1

HCID 20317399Methyl 7-[2-(3-Hydroxy-4-propoxybutyl)-1,4-dioxo-3-thiazolidinyl]heptanoate

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

A solution of diazomethane (approximately 2.5 g., 0.06 mole) in ether (100 ml.) is slowly added to a solution of 7-[2-(3-hydroxy-4-propoxybutyl)-1,4-dioxo-3-thiazolidinyl]heptanoic acid (11.3 g., 0.03 mole) in ether (50 ml.) with stirring and cooling (0° to 5° C.). The resulting solution is allowed to warm to and stand at room temperature for 4 hours. After destroying excess diazomethane with acetic acid, the reaction solution is washed with 5% sodium bicarbonate solution and water, dried over sodium sulfate, and filtered. In vacuo evaporation of the filtrate leaves the title compound as an essentially colorless, viscous oil.

후처리

  1. temperaturecooling (0° to 5° C.)
  2. temperatureto warm to and
  3. customAfter destroying excess diazomethane with acetic acid
  4. washthe reaction solution is washed with 5% sodium bicarbonate solution and water
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. customIn vacuo evaporation of the filtrate

출처 및 근거

ORD 기록
ord-af612ee5b1b44eeb88933c106b480f2e
출처 데이터셋
uspto-grants-1978_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04102888

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