Putrescine → N,N'-(butane-1,4-diyl)bis(4-(6,8-dichloro-2-methyl-1,2,3,4-tetrahydroisoquinolin-4-yl)benzenesulfonamide)

HRID 1479363

反応式

[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[C:10]([Cl:12])[CH:11]=1)[CH2:8][N:7]([CH3:13])[CH2:6][CH:5]2[C:14]1[CH:19]=[CH:18][C:17]([S:20](Cl)(=[O:22])=[O:21])=[CH:16][CH:15]=1.C[CH2:25][N:26]([CH:30]([CH3:32])C)[CH:27]([CH3:29])C.[CH2:33]([NH2:38])[CH2:34][CH2:35][CH2:36][NH2:37]>C(Cl)(Cl)Cl>[CH2:33]([NH:38][S:20]([C:17]1[CH:18]=[CH:19][C:14]([CH:32]2[C:4]3[C:29](=[C:10]([Cl:12])[CH:11]=[C:2]([Cl:1])[CH:3]=3)[CH2:27][N:26]([CH3:25])[CH2:30]2)=[CH:15][CH:16]=1)(=[O:22])=[O:21])[CH2:34][CH2:35][CH2:36][NH:37][S:20]([C:17]1[CH:18]=[CH:19][C:14]([CH:5]2[C:4]3[C:9](=[C:10]([Cl:12])[CH:11]=[C:2]([Cl:1])[CH:3]=3)[CH2:8][N:7]([CH3:13])[CH2:6]2)=[CH:15][CH:16]=1)(=[O:22])=[O:21]

参加物

実験手順

To a solution of 4-(6,8-dichloro-2-methyl-1,2,3,4-tetrahydroisoquinolin-4-yl)benzene-1-sulfonyl chloride (intermediate 10.6) (150 mg, 0.353 mmol) in chloroform (0.706 mL) was added DIEA (182 mg, 1.412 mmol) and a solution of butane-1,4-diamine (15.5 mg, 0.176 mmol) in chloroform (0.176 mL). The reaction was stirred overnight at which point the solvent was removed and the resulting residue brought up in 50% IPA/H2O. Purification by preparative HPLC gave the title compound (18.4 mg) as a TFA salt. 1H-NMR (400 MHz, CD3OD): δ7.86 (d, 4H), 7.53 (s, 2H), 7.45 (d, 4H), 6.84 (s, 2H), 4.73 (m, 3H), 4.46 (d, 2H), 3.86 (dd, 2H), 3.57 (t, 2H), 3.12 (s, 6H), 2.84 (m, 4H), 1.41 (m, 4H). MS (m/z): 797.15 (M+H).

後処理

customwas removed
customPurification by preparative HPLC

出典と根拠

ORDレコード: ord-a0d2436a43a24e1f95f38d960e740d86
出典データセット: uspto-grants-2016_08
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US09408840B2

反応式

参加物

反応物 3

生成物 1

試薬・触媒・溶媒 1

実験手順

後処理

出典と根拠

関連ノート