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Sodium hydride → N-Boc-O-(2,2,5,5-tetramethyl-1-cyclopentyl)-1-amino-1-hydroxymethylcyclopropane

HRID 1731685
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HRID 1731685 반응식
[CH3:1][C:2]1([CH3:10])[CH2:6][CH2:5][C:4]([CH3:8])([CH3:7])[CH:3]1[OH:9].[H-].[Na+].C1OCCOCCOCCOCCOCCOC1.CCOCC.S(O)(=O)(=O)C.[C:41]([NH:48][C:49]1([CH2:52]O)[CH2:51][CH2:50]1)([O:43][C:44]([CH3:47])([CH3:46])[CH3:45])=[O:42]>C(#N)C.O1CCCC1>[C:41]([NH:48][C:49]1([CH2:52][O:9][CH:3]2[C:4]([CH3:8])([CH3:7])[CH2:5][CH2:6][C:2]2([CH3:10])[CH3:1])[CH2:51][CH2:50]1)([O:43][C:44]([CH3:47])([CH3:46])[CH3:45])=[O:42]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 24758Sodium hydrideHCID 5516962,2,5,5-Tetramethylcyclopentan-1-olHCID 20092326Ethoxyethane;1,4,7,10,13,16-hexaoxacyclooctadecaneHCID 20165745N-Boc-1-amino-1-hydroxymethylcyclopropane mesylate

생성물 1

HCID 20165730N-Boc-O-(2,2,5,5-tetramethyl-1-cyclopentyl)-1-amino-1-hydroxymethylcyclopropane

시약·촉매·용매 2

HCID 6342
Acetonitrile
용매
HCID 8028Tetrahydrofuran용매2회

실험 절차

2,2,5,5-Tetramethyl-1-cyclopentanol is added to a dry flask under argon at 0° C. Dry tetrahydrofuran is added with a syringe. Sodium hydride (60% dispersion in oil) is added quickly in one portion and the contents of the flask are stirred for one hour at room temperature. A 10 mM solution of 18-crown-6- ether in acetonitrile is added with a syringe and the flask cooled to 0° C. A tetrahydrofuran solution of N-Boc-1-amino-1-hydroxymethylcyclopropane mesylate is added with vigorous stirring over a 10 minute period. After completion of the reaction, as judged by thin layer chromatography, it is quenched with dimethyl sulfate, poured into saturated ammonium chloride and extracted with ethyl acetate. The organic layer is dried over MgSO4 and evaporated to yield N-Boc-O-(2,2,5,5-tetramethyl-1-cyclopentyl)-1-amino-1-hydroxymethylcyclopropane.

후처리

  1. temperaturethe flask cooled to 0° C
  2. stirringwith vigorous stirring over a 10 minute period
  3. customAfter completion of the reaction
  4. customis quenched with dimethyl sulfate
  5. additionpoured into saturated ammonium chloride
  6. extractionextracted with ethyl acetate
  7. dry with materialThe organic layer is dried over MgSO4
  8. customevaporated

출처 및 근거

ORD 기록
ord-fc2ab26bae4748f5ac9058042d4d93d0
출처 데이터셋
uspto-grants-1986_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04622418

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