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Water → Pentanoic acid [6-benzyl-4-(2-chloro-phenyl)-5,6,7,8-tetrahydro-pyrido[4,3-d]pyrimidin-2-yl]-amide

HRID 1020007
ノート
印刷プレビュー

反応式

HRID 1020007 の反応式
CO[C:3]([CH:5]1[C:10](=O)[CH2:9][CH2:8][N:7]([CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH2:6]1)=O.[ClH:19].[NH2:20][C:21]([NH2:23])=[NH:22].[C:24](=[O:27])([O-])[O-].[K+].[K+].O>CN(C=O)C.CO>[CH2:12]([N:7]1[CH2:8][CH2:9][C:10]2[N:22]=[C:21]([NH:23][C:24](=[O:27])[CH2:3][CH2:5][CH2:10][CH3:9])[N:20]=[C:3]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[Cl:19])[C:5]=2[CH2:6]1)[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][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

7

反応物 4

HCID 962WaterHCID 5742Guanidine HydrochlorideHCID 11430Potassium CarbonateHCID 107480Methyl 1-benzyl-4-oxo-3-piperidinecarboxylate

生成物 1

HCID 46937260Pentanoic acid [6-benzyl-4-(2-chloro-phenyl)-5,6,7,8-tetrahydro-pyrido[4,3-d]pyrimidin-2-yl]-amide収率 87%

試薬・触媒・溶媒 2

HCID 887
Methanol
溶媒
HCID 6228Dimethylformamide溶媒

実験手順

Methyl-1-benzyl-4-oxo-3-piperidine carboxylate (5.68 g., 20 mmoles) and guanidine hydrochloride (2.0 g., 21 mmoles) were suspended and stirred in dry DMF (45 mls) before potassium carbonate (5.68 g., 41 mmoles) was added portionwise over 15 minutes. The reaction mixture was poured onto cold water (750 mls) to release a white/beige solid which was rapidly stirred for 30 minutes. The solid was filtered washed with water (100 mls) and dried in a vacuum desiccator. The product was then slurried in ether (150 mls), filtered and dried in vacuo overnight, to leave an off-white solid (4.46 g., 87% yield). Single spot by tlc (MeOH, Rf 0.66), LC-MS (retention 2.20 mins., mass 257 M+H).

後処理

  1. additionwas added portionwise over 15 minutes
  2. filtrationThe solid was filtered
  3. washwashed with water (100 mls)
  4. customdried in a vacuum desiccator
  5. filtrationfiltered
  6. customdried in vacuo overnight
  7. customto leave an off-white solid (4.46 g., 87% yield)

出典と根拠

ORDレコード
ord-52fae9d42e2e45bc97532e3e142d46a0
出典データセット
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08716302B2

反応ノート

読み込み中…

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