Ethyl Acetate → Methyl 3-(benzyloxy)-4-oxo-6,7,8,9-tetrahydro-4H-pyrido[1,2-a]pyrimidine-2-carboxylate

HRID 2219042ノート

反応式

HRID 2219042 の反応式
Cl.[NH:2]=[C:3]1[CH2:8][CH2:7][CH2:6][CH2:5][NH:4]1.[CH2:9]([O:16][CH:17]([C:22](=O)[C:23]([O:25][CH3:26])=[O:24])[C:18](OC)=[O:19])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.C1CCN2C(=NCCC2)CC1.CCOC(C)=O>CO>[CH2:9]([O:16][C:17]1[C:18](=[O:19])[N:4]2[CH2:5][CH2:6][CH2:7][CH2:8][C:3]2=[N:2][C:22]=1[C:23]([O:25][CH3:26])=[O:24])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

参加物

6

反応物 4

HCID 8857Ethyl AcetateHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 59771073Dimethyl 2-(benzyloxy)-3-oxosuccinateHCID 178479080HCID 178479080、化合物

生成物 1

HCID 59771042Methyl 3-(benzyloxy)-4-oxo-6,7,8,9-tetrahydro-4H-pyrido[1,2-a]pyrimidine-2-carboxylate

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Commercially available 2-iminopiperidine hydrochloride (1.5 eq) was added at room temperature to a solution of oxosuccinate prepared in Step 1b (1 eq) in MeOH. After dropwise addition of neat DBU (4.5 eq), the reaction mixture was stirred for 2 days. Evaporation of the solvent gave a residue that was taken into EtOAc and washed with 1N HCl and brine; the organic layer was dried on Na2SO4 and the solvent removed. The crude was used without further purification.

後処理

  1. customEvaporation of the solvent
  2. customgave a residue that
  3. washwashed with 1N HCl and brine
  4. customthe organic layer was dried on Na2SO4
  5. customthe solvent removed
  6. customThe crude was used without further purification

出典と根拠

ORDレコード
ord-9d22f86b9a6c4d4baf3b27f9553a02c2
出典データセット
uspto-grants-2008_08
特許番号
US07414045B2

反応ノート

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