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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
ノート
印刷プレビュー

反応式

HRID 1434927 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-cd8ece670e464abf89f388607553056d
出典データセット
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07615562B2

反応ノート

読み込み中…

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