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Aluminium lithium hydride → 4-{5-[5-Methyl-2-(2,2,6,6-tetramethyl-piperidin-4-ylamino)-pyrimidin-4-yl]-thiophen-2-yl}-butan-1-ol

HRID 1434927
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HRID 1434927 반응식
C[O:2][C:3](=O)[CH2:4][CH2:5][CH2:6][C:7]1[S:8][C:9]([C:12]2[C:17]([CH3:18])=[CH:16][N:15]=[C:14]([NH:19][CH:20]3[CH2:25][C:24]([CH3:27])([CH3:26])[NH:23][C:22]([CH3:29])([CH3:28])[CH2:21]3)[N:13]=2)=[CH:10][CH:11]=1.[H-].[H-].[H-].[H-].[Li+].[Al+3]>C1COCC1>[CH3:18][C:17]1[C:12]([C:9]2[S:8][C:7]([CH2:6][CH2:5][CH2:4][CH2:3][OH:2])=[CH:11][CH:10]=2)=[N:13][C:14]([NH:19][CH:20]2[CH2:21][C:22]([CH3:28])([CH3:29])[NH:23][C:24]([CH3:27])([CH3:26])[CH2:25]2)=[N:15][CH:16]=1
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참가 물질

4

반응물 2

HCID 21226445Aluminium lithium hydrideHCID 579361484-{5-[5-Methyl-2-(2,2,6,6-tetramethyl-piperidin-4-ylamino)-pyrimidin-4-yl]-thiophen-2-yl}-butyric acid methyl ester

생성물 1

HCID 112004814-{5-[5-Methyl-2-(2,2,6,6-tetramethyl-piperidin-4-ylamino)-pyrimidin-4-yl]-thiophen-2-yl}-butan-1-ol

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

The ester from Step B (37 mg, 0.09 mmol) was dissolved in 1 ml of THF and LAH (1M in THF, 0.22 ml, 0.22 mmol) was added. After 30 minutes, the mixture was quenched with water and extracted with ether. The organic layers were washed with brine, dried over sodium sulfate and evaporated. The crude product was purified by preparative HPLC. Yield: 15 mg (43%).

후처리

  1. customthe mixture was quenched with water
  2. extractionextracted with ether
  3. washThe organic layers were washed with brine
  4. dry with materialdried over sodium sulfate
  5. customevaporated
  6. customThe crude product was purified by preparative HPLC

출처 및 근거

ORD 기록
ord-cd8ece670e464abf89f388607553056d
출처 데이터셋
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07615562B2

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