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Lithium Hydroxide → HCID 9799185, 화합물

HRID 1075621
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HRID 1075621 반응식
[CH3:1][C:2]1([C:19]2[CH:29]=[CH:28][C:22]([C:23]([O:25]CC)=[O:24])=[CH:21][CH:20]=2)[CH2:6][O:5][C:4]2[CH:7]=[C:8]3[C:13](=[CH:14][C:3]1=2)[C:12]([CH3:16])([CH3:15])[CH2:11][CH2:10][C:9]3([CH3:18])[CH3:17].[OH-].[Na+].[OH-].[Li+].C1COCC1>O.CO>[CH3:1][C:2]1([C:19]2[CH:20]=[CH:21][C:22]([C:23]([OH:25])=[O:24])=[CH:28][CH:29]=2)[CH2:6][O:5][C:4]2[CH:7]=[C:8]3[C:13](=[CH:14][C:3]1=2)[C:12]([CH3:15])([CH3:16])[CH2:11][CH2:10][C:9]3([CH3:17])[CH3:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 3939Lithium HydroxideHCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 70193470HCID 70193470, 화합물

생성물 1

HCID 9799185HCID 9799185, 화합물

시약·촉매·용매 2

HCID 887Methanol용매
HCID 962
Water
용매

실험 절차

A mixture of ethyl 4-(3,5,5,8,8-pentamethyl-2,3,5,6,7,8-hexahydronaphtho[2,3-b]furan-3-yl)benzoate (200 mg, 0.5 mmol), sodium hydroxide (100 mg, 2.4 mmol) and lithium hydroxide (100 mg, 2.4 mmol) in 5 ml of a solution of THF, methanol and water (5/1/1) was heated under reflux for 24 h. The reaction medium was concentrated in a rotary evaporator under vacuum at 40° C. After adding 5 ml of water and 5 ml of ethyl ether and acidifying with a concentrated hydrochloric acid solution to pH 1, the organic phase was washed twice with 5 ml of water, dried over magnesium sulfate and concentrated in a rotary evaporator under vacuum at 40° C. The solids obtained were washed with heptane.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 24 h
  3. concentrationThe reaction medium was concentrated in a rotary evaporator under vacuum at 40° C
  4. additionAfter adding 5 ml of water and 5 ml of ethyl ether and acidifying with a concentrated hydrochloric acid solution to pH 1
  5. washthe organic phase was washed twice with 5 ml of water
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated in a rotary evaporator under vacuum at 40° C
  8. customThe solids obtained
  9. washwere washed with heptane

출처 및 근거

ORD 기록
ord-54d5eb7c3b6d4cb2a7307803342a0d11
출처 데이터셋
uspto-grants-1999_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05905088

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