Cyclooctylamine → HCID 19938097, 화합물

HRID 36441

반응식

HRID 36441 반응식
[CH:1]1([NH2:9])[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[CH3:10][O:11][CH2:12][O:13][C:14]1[CH:19]=[CH:18][C:17]([CH:20]([C:29]2[CH:34]=[CH:33][C:32]([O:35][CH2:36][O:37][CH3:38])=[CH:31][CH:30]=2)[C:21]2[CH:28]=[CH:27][CH:26]=[CH:25][C:22]=2[CH:23]=O)=[CH:16][CH:15]=1.[BH4-].[Na+]>C(O)C>[CH:1]1([NH:9][CH2:23][C:22]2[CH:25]=[CH:26][CH:27]=[CH:28][C:21]=2[CH:20]([C:17]2[CH:16]=[CH:15][C:14]([O:13][CH2:12][O:11][CH3:10])=[CH:19][CH:18]=2)[C:29]2[CH:30]=[CH:31][C:32]([O:35][CH2:36][O:37][CH3:38])=[CH:33][CH:34]=2)[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

참가 물질

5

반응물 3

HCID 2903CyclooctylamineHCID 4311764Sodium borohydrideHCID 19938143HCID 19938143, 화합물

생성물 1

HCID 19938097HCID 19938097, 화합물수율 89.4%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

In 50 ml of ethanol was dissolved 0.69 g of cyclooctylamine. To the solution was added 1.96 g of 2-[bis(4-methoxymethoxyphenyl)methyl]benzaldehyde obtained by Reference Example 3, and the mixture was stirred overnight. Then, 0.85 g of sodium borohydride was added thereto, and the reaction mixture was stirred for 2 hours. Thereafter, the solvent was evaporated under reduced pressure, and water was added to the residue. The aqueous mixture was extracted with chloroform, and the organic layer was separated. The aqueous layer was extracted with chloroform, and the organic layer was combined and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel chromatography to afford 2.25 g of the desired product (Compound 77) as an oily matter.

후처리

  1. customobtained by Reference Example 3
  2. stirringthe reaction mixture was stirred for 2 hours
  3. customThereafter, the solvent was evaporated under reduced pressure, and water
  4. additionwas added to the residue
  5. extractionThe aqueous mixture was extracted with chloroform
  6. customthe organic layer was separated
  7. extractionThe aqueous layer was extracted with chloroform
  8. dry with materialdried over anhydrous magnesium sulfate
  9. customThe solvent was evaporated under reduced pressure
  10. customthe residue was purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-c97e50d097fd4a3aae5ba7b68380f0cf
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05413997

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