Diethyl Ether → HCID 24758399、化合物

HRID 889588

反応式

HRID 889588 の反応式
N1CCC(CC2NC3=NC=CC=C3C=2)C1.C(OC(N1CCCC(C2C3C(=NC=CC=3)NC=2)C1)=O)(C)(C)C.CCOCC.[CH3:43][N:44]1[CH2:49][CH2:48][CH2:47][CH:46]([C:50]2[NH:58][C:53]3=[N:54][CH:55]=[CH:56][CH:57]=[C:52]3[CH:51]=2)[CH2:45]1>CO.C(N(CC)CC)C>[CH3:43][N:44]1[CH2:49][CH2:48][CH:47]([CH2:46][C:50]2[NH:58][C:53]3=[N:54][CH:55]=[CH:56][CH:57]=[C:52]3[CH:51]=2)[CH2:45]1

参加物

6

反応物 4

HCID 3283Diethyl EtherHCID 24758035HCID 24758035、化合物HCID 24758401HCID 24758401、化合物HCID 58172463HCID 58172463、化合物

生成物 1

HCID 24758399HCID 24758399、化合物

試薬・触媒・溶媒 1

HCID 22728368Triethylamine methanol溶媒

実験手順

Compound 66 (0.3 g, 1.49 mmol) was converted to compound 67, using the methodology described for compound 9. Yield 0.362 g (80.7%). (TLC ether Rf 0.11), which was used as such to generate the title compound (68) using the methodology as described for compound 28. (Yield 0.17 g, 65%), mp 96-97° C. 1H-NMR (400 MHz, CDCl3): δ N1—H invisible, 8.16 (dd, J=5 Hz, 2 Hz, 1H), 7.77 (dd, J=8 Hz, 2 Hz, 1H), 6.98 (dd, J=8 Hz, 5 Hz, 1H), 6.16 (bs, 1H), 2.92-2.84 (m, 2H), 2.76-2.64 (m, 2H), 2.62-2.50 (m, 2H), 2.34 (s, 3H), 2.40-2.31 (m, 1H), 2.11-2.01 (m, 1H), 1.63-1.53 (m, 1H). (TLC MeOH/triethylamine (97/3) Rf 0.2).

出典と根拠

ORDレコード
ord-31a9be0fe2d8429181617fb2836d8ab4
出典データセット
uspto-grants-2012_08
特許番号
US08252930B2

関連ノート

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