Hydrochloric Acid → HCID 66742899、化合物

反応式

[CH3:1][N:2]1[C:7]2[N:8]([CH3:16])[CH:9]=[C:10]([CH2:11][C:12]([O:14]C)=[O:13])[C:6]=2[C:5](=[O:17])[N:4]([CH3:18])[C:3]1=[O:19].Cl>>[CH3:1][N:2]1[C:7]2[N:8]([CH3:16])[CH:9]=[C:10]([CH2:11][C:12]([OH:14])=[O:13])[C:6]=2[C:5](=[O:17])[N:4]([CH3:18])[C:3]1=[O:19]

参加物

反応物 2

HCID 313Hydrochloric Acid

HCID 123561205HCID 123561205、化合物

生成物 1

HCID 66742899HCID 66742899、化合物

実験手順

A mixture of Step 4 intermediate (130 mg, 0.491 mmol) and concentrated hydrochloric acid (4 mL) was heated at 60° C. for 2 h. The excess of hydrochloric acid was evaporated under reduced pressure and the residue obtained was purified by silica gel column chromatography using 5% methanol in chloroform to obtain 94 mg of the product as a white solid; 1H NMR (δ ppm, 300 MHz, DMSO-d6) 3.21 (s, 3H), 3.65-3.72 (m, 8H), 6.29 (s, 1H), 12.62 (br s, 1H); APCI-MS (m/z) 252.38 (M+H)+.

後処理

customThe excess of hydrochloric acid was evaporated under reduced pressure
customthe residue obtained
customwas purified by silica gel column chromatography

出典と根拠

ORDレコード: ord-09536db49b4847c8b2f18bf23641cd87
出典データセット: uspto-grants-2015_04
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US09000159B2

反応ノート

読み込み中…

参加物