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Triethylamine → HCID 178482373、化合物

HRID 1801562
ノート
印刷プレビュー

反応式

HRID 1801562 の反応式
Cl.[NH:2]1[CH2:7][CH2:6][CH:5]([C:8]2[N:13]=[C:12]([N:14]3[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]3)[N:11]=[C:10]([OH:20])[CH:9]=2)[CH2:4][CH2:3]1.[CH3:21][NH:22][C:23]1[N:28]=[CH:27][C:26]([CH:29]=O)=[CH:25][N:24]=1.C(N(CC)CC)C.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>C(O)(=O)C.ClCCl>[CH3:21][NH:22][C:23]1[N:28]=[CH:27][C:26]([CH2:29][N:2]2[CH2:7][CH2:6][CH:5]([C:8]3[N:13]=[C:12]([N:14]4[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19]4)[N:11]=[C:10]([OH:20])[CH:9]=3)[CH2:4][CH2:3]2)=[CH:25][N:24]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8471TriethylamineHCID 31609752-(Methylamino)pyrimidine-5-carbaldehydeHCID 5049666Sodium triacetoxyborohydrideHCID 178479621HCID 178479621、化合物

生成物 1

HCID 178482373HCID 178482373、化合物収率 83.1%

試薬・触媒・溶媒 2

HCID 176Acetic Acid
触媒
HCID 6344Dichloromethane溶媒

実験手順

A mixture of 6-piperidin-4-yl-2-piperidin-1-yl-pyrimidin-4-ol, hydrochloride salt (2.0 mmol), 2-methylaminopyrimidine-5-carbaldehyde (2.6 mmol), triethylamine (4.0 mmol) and 3 drops of acetic acid in dry dichloromethane (20 mL) was stirred at room temperature for 3 hours. Then sodium triacetoxyborohydride (6.0 mmol) was added in portions and stirring was continued for 48 hours (monitored by TLC). The mixture was quenched with saturated aqueous sodium bicarbonate solution (20 mL), and the product was extracted with dichloromethane (2×10 mL). The extracts were washed with brine and dried over sodium sulfate. The solvent was evaporated in vacuo to give a crude product. Purification via column chromatography (silica gel, ethyl acetate/hexane) afforded 6-[1-(2-methylaminopyrimidin-5-ylmethyl)-piperidin-4-yl]-2-piperidin-1-yl-pyrimidin-4-ol (Compound IIc, 637 mg, 83%).

後処理

  1. stirringstirring
  2. waitwas continued for 48 hours
  3. customThe mixture was quenched with saturated aqueous sodium bicarbonate solution (20 mL)
  4. extractionthe product was extracted with dichloromethane (2×10 mL)
  5. washThe extracts were washed with brine
  6. dry with materialdried over sodium sulfate
  7. customThe solvent was evaporated in vacuo
  8. customto give a crude product
  9. customPurification via column chromatography (silica gel, ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-d58d3e82003d49929b2016c145809bbf
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08349833B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート