N1,N1-bis(2-methoxyethyl)-3-methylbutane-1,3-diamine → 2((4-(bis(2-methoxyethyl)amino)-2-methylbutan-2-yl)amino)-8-iodo-3-methylquinazolin-4(3H)-one

HRID 1056358ノート

反応式

HRID 1056358 の反応式
[CH3:1][O:2][CH2:3][CH2:4][N:5]([CH2:12][CH2:13][O:14][CH3:15])[CH2:6][CH2:7][C:8]([CH3:11])([NH2:10])[CH3:9].[I:16][C:17]1[CH:18]=[CH:19][CH:20]=[C:21]2[C:26]=1[N:25]=[C:24](S(C)=O)[N:23]([CH3:30])[C:22]2=[O:31]>CC(O)(C)C>[CH3:15][O:14][CH2:13][CH2:12][N:5]([CH2:4][CH2:3][O:2][CH3:1])[CH2:6][CH2:7][C:8]([NH:10][C:24]1[N:23]([CH3:30])[C:22](=[O:31])[C:21]2[C:26](=[C:17]([I:16])[CH:18]=[CH:19][CH:20]=2)[N:25]=1)([CH3:11])[CH3:9]

参加物

4

反応物 2

HCID 64679532N1,N1-bis(2-methoxyethyl)-3-methylbutane-1,3-diamineHCID 897821678-iodo-3-methyl-2-(methylsulfinyl)quinazolin-4(3H)-one

生成物 1

HCID 897821272((4-(bis(2-methoxyethyl)amino)-2-methylbutan-2-yl)amino)-8-iodo-3-methylquinazolin-4(3H)-one収率 183.4%

試薬・触媒・溶媒 1

HCID 6386tert-Butanol溶媒

反応条件

温度
120 °C

実験手順

A glass microwave reaction vessel was charged with N1,N1-bis(2-methoxyethyl)-3-methylbutane-1,3-diamine (50 mg, 0.229 mmol) and 8-iodo-3-methyl-2-(methylsulfinyl)quinazolin-4(3H)-one (700b; 80 mg, 0.229 mmol) in tBuOH (0.5 mL). The reaction mixture was stirred and heated in a Initiator microwave reactor (Personal Chemistry, Biotage AB, Inc.) at 120° C. for 45 min. Similarly another two batches (50 mg and 170 mg) were carried out. The three batches were combined and the solvent was removed. The residue was purified with silica gel chromatography (eluted with 0-5% MeOH in DCM) to give 2((4-(bis(2-methoxyethyl)amino)-2-methylbutan-2-yl)amino)-8-iodo-3-methylquinazolin-4(3H)-one (210 mg, 0.42 mmol). MS (ESI, pos. ion) m/z: 503 (M+1).

後処理

  1. customA glass microwave reaction vessel
  2. customthe solvent was removed
  3. customThe residue was purified with silica gel chromatography (eluted with 0-5% MeOH in DCM)

出典と根拠

ORDレコード
ord-3f71d11e621148d7b6753e4cbcbbb4d4
出典データセット
uspto-grants-2016_07
特許番号
US09394297B2

反応ノート

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