Water → HCID 64842474, 화합물

HRID 2360713노트

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HRID 2360713 반응식
[CH2:1]([N:8]1[CH2:17][C:16]([CH3:19])([CH3:18])[NH:15][C:14](=O)[C:9]21[CH2:13][CH2:12][CH2:11][CH2:10]2)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].Cl[Si](C)(C)C.O>C1COCC1>[CH2:1]([N:8]1[CH2:17][C:16]([CH3:19])([CH3:18])[NH:15][CH2:14][C:9]21[CH2:10][CH2:11][CH2:12][CH2:13]2)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 6397ChlorotrimethylsilaneHCID 21226445Aluminium lithium hydrideHCID 866803356-Benzyl-8,8-dimethyl-6,9-diaza-spiro[4.5]decan-10-one

생성물 1

HCID 64842474HCID 64842474, 화합물수율 93%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

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온도
55 °C

실험 절차

Under Argon atmosphere to a solution of 10.78 g of 6-benzyl-8,8-dimethyl-6,9-diaza-spiro[4.5]decan-10-one in 160 ml of THF 33 ml of a 2.4 M solution of lithium aluminium hydride in THF were slowly added. The reaction was heated to 55° C., and 5 ml of chlorotrimethylsilane were added dropwise. The reaction was kept at 55-60° C. for 2.5 h and then cooled to 0° C. 16 ml of water were added dropwise, and THF was added. The mixture was filtered by suction over celite and the filtrate was concentrated in vacuo. The product was precipitated by treatment with methyl tert-butyl ether. 9.47 g (93%) of the title compound were obtained.

후처리

  1. temperaturecooled to 0° C
  2. filtrationThe mixture was filtered by suction over celite
  3. concentrationthe filtrate was concentrated in vacuo
  4. customThe product was precipitated by treatment with methyl tert-butyl ether

출처 및 근거

ORD 기록
ord-d656a166e42446d19edf28ab71225e61
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08686150B2

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