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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Water → HCID 86692469, 화합물

HRID 1748520
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HRID 1748520 반응식
[OH-].[Na+].O.C([O:6][C:7]([C:9]1([C:19]2[CH:24]=[CH:23][C:22]([Br:25])=[CH:21][N:20]=2)[CH2:18][CH2:17][C:12]2([O:16][CH2:15][CH2:14][O:13]2)[CH2:11][CH2:10]1)=[O:8])C>CO.O1CCCC1>[Br:25][C:22]1[CH:23]=[CH:24][C:19]([C:9]2([C:7]([OH:8])=[O:6])[CH2:10][CH2:11][C:12]3([O:16][CH2:15][CH2:14][O:13]3)[CH2:17][CH2:18]2)=[N:20][CH:21]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 86692455HCID 86692455, 화합물

생성물 1

HCID 86692469HCID 86692469, 화합물수율 93.5%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

4N Aqueous solution of sodium hydroxide (5 ml) and water (5 ml) were added to a solution of 8-(5-bromopyridin-2-yl)-1,4-dioxaspiro[4,5]decane-8-carboxylic acid ethyl ester (1.0 g) described in Reference Example 81(2) in methanol (10 ml) and tetrahydrofuran (10 ml), and stirred at 80° C. for eight hours. After completion of the reaction, the organic solvent was evaporated and the aqueous layer was washed with diethyl ether. Concentrated hydrochloric acid was added to the aqueous layer under ice cooling, pH was adjusted to 4-5, and extracted with chloroform. The organic layer was dried over anhydrous sodium sulfate and concentrated to give 8-(5-bromopyridin-2-yl)-1,4-dioxaspiro[4,5]decane-8-carboxylic acid (864 mg) as a colorless solid.

후처리

  1. customAfter completion of the reaction
  2. customthe organic solvent was evaporated
  3. washthe aqueous layer was washed with diethyl ether
  4. additionConcentrated hydrochloric acid was added to the aqueous layer under ice cooling
  5. extractionextracted with chloroform
  6. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-5beaceb1fe304717b0f6fe8f314aa667
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09150555B2

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