Dicyclohexylcarbodiimide → 3-[[[4,5-Bis(phenylmethoxy)-2-pyridinyl]carbonyl]amino]-tetrahydro-2-oxo-1(2H)-pyrimidinecarboxamide

HRID 2351091ノート

反応式

HRID 2351091 の反応式
[NH2:1][N:2]1[CH2:7][CH2:6][CH2:5][N:4]([C:8]([NH2:10])=[O:9])[C:3]1=[O:11].C1(N=C=NC2CCCCC2)CCCCC1.ON1C2C=CC=CC=2N=N1.[C:37]1([CH2:43][O:44][C:45]2[C:50]([O:51][CH2:52][C:53]3[CH:58]=[CH:57][CH:56]=[CH:55][CH:54]=3)=[CH:49][N:48]=[C:47]([C:59](O)=[O:60])[CH:46]=2)[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1>CN(C)C=O>[C:37]1([CH2:43][O:44][C:45]2[C:50]([O:51][CH2:52][C:53]3[CH:54]=[CH:55][CH:56]=[CH:57][CH:58]=3)=[CH:49][N:48]=[C:47]([C:59]([NH:1][N:2]3[CH2:7][CH2:6][CH2:5][N:4]([C:8]([NH2:10])=[O:9])[C:3]3=[O:11])=[O:60])[CH:46]=2)[CH:38]=[CH:39][CH:40]=[CH:41][CH:42]=1

参加物

6

反応物 4

HCID 10868DicyclohexylcarbodiimideHCID 757711-HydroxybenzotriazoleHCID 141825074,5-bis(phenylmethoxy)-2-Pyridinecarboxylic acidHCID 198480103-Amino-2-oxotetrahydropyrimidine-1(2H)-carboxamide

生成物 1

HCID 198480113-[[[4,5-Bis(phenylmethoxy)-2-pyridinyl]carbonyl]amino]-tetrahydro-2-oxo-1(2H)-pyrimidinecarboxamide収率 91.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 3-aminotetrahydro-2-oxo-1(2H)-pyrimidinecarboxamide (10 g, 63.2 mmol) in 350 ml N,N-dimethylformamide were added dicyclohexylcarbodiimide (15.7 g, 75.9 mmol), N-hydroxybenzotriazole (0.97 g, 6.32 mmol) and 4,5-bis(phenylmethoxy)-2-pyridinecarboxylic acid (21.2 g, 63.2 mmol) and the mixture was stirred overnight at room temperature. Dicyclohexylurea (13.6 g) was filtered off and the solvent was removed in vacuo. Trituration of the residue with ether gave 27.5 g of the desired product, melting point 192°-195° C.

後処理

  1. filtrationDicyclohexylurea (13.6 g) was filtered off
  2. customthe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-4b422f76e06d495ca7961a7988887f21
出典データセット
uspto-grants-1989_10
特許番号
US04871841

反応ノート

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