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Tetrahydro-4H-pyran-4-one → 6-chloro-5-methyl-1-[1-(tetrahydro-2H-pyran-4-yl)-4-piperidinyl]-1,3-dihydro-2H-benzimidazol-2-one

HRID 2064205
ノート
印刷プレビュー

反応式

HRID 2064205 の反応式
Cl.[Cl:2][C:3]1[C:4]([CH3:19])=[CH:5][C:6]2[NH:10][C:9](=[O:11])[N:8]([CH:12]3[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]3)[C:7]=2[CH:18]=1.[O:20]1[CH2:25][CH2:24][C:23](=O)[CH2:22][CH2:21]1.[BH3-]C#N.[Na+]>CO>[Cl:2][C:3]1[C:4]([CH3:19])=[CH:5][C:6]2[NH:10][C:9](=[O:11])[N:8]([CH:12]3[CH2:13][CH2:14][N:15]([CH:23]4[CH2:24][CH2:25][O:20][CH2:21][CH2:22]4)[CH2:16][CH2:17]3)[C:7]=2[CH:18]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 121599Tetrahydro-4H-pyran-4-oneHCID 5003444Sodium cyanoborohydrideHCID 691281886-Chloro-5-methyl-1-(4-piperidinyl)-1,3-dihydro-2H-benzimidazol-2-one hydrochloride

生成物 1

HCID 160710146-chloro-5-methyl-1-[1-(tetrahydro-2H-pyran-4-yl)-4-piperidinyl]-1,3-dihydro-2H-benzimidazol-2-one

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

6-Chloro-5-methyl-1-(4-piperidinyl)-1,3-dihydro-2H-benzimidazol-2-one hydrochloride (D9) (˜0.2 mmol, 60 mg), Ti(iPrO)4 (2 eq., 0.400 mmol, 0.130 ml), tetrahydro-4H-pyran-4-one (2 eq., 0.400 mmol, 40 ul) were stirred together at room temperature for one hour; dry MeOH (2 ml) followed by NaBH3CN (2 eq., ˜30 mgs) were added and the mixture was stirred under argon at room temperature for 3 hours. The crude mixture was subsequently quenched with water (5 ml) and it was firstly purified by SCX followed by chromatography (methanol-NH3-dichloromethane) to yield 6-chloro-5-methyl-1-[1-(tetrahydro-2H-pyran-4-yl)-4-piperidinyl]-1,3-dihydro-2H-benzimidazol-2-one, 10 mg, 14%, M++H=350, which was converted into the hydrochloride salt using 1M HCl in diethyl ether.

後処理

  1. additionwere added
  2. customThe crude mixture was subsequently quenched with water (5 ml) and it
  3. customwas firstly purified by SCX

出典と根拠

ORDレコード
ord-4b5b942c28c24a2e836451d65691894c
出典データセット
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08288412B2

反応ノート

読み込み中…

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