Diisopropylethylamine → HCID 58116988、化合物

HRID 38611ノート

反応式

HRID 38611 の反応式
Cl.[Cl:2][C:3]1[C:8]([Cl:9])=[CH:7][C:6]([NH:10][C:11]2[C:12]3[C:19]4[CH2:20][CH2:21][NH:22][CH2:23][C:18]=4[S:17][C:13]=3[N:14]=[CH:15][N:16]=2)=[CH:5][C:4]=1[OH:24].Cl.[CH3:26][N:27]([CH:34]([CH3:36])[CH3:35])[CH2:28]/[CH:29]=[CH:30]/[C:31](O)=[O:32].CCN(C(C)C)C(C)C.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F>CN(C=O)C>[Cl:2][C:3]1[C:8]([Cl:9])=[CH:7][C:6]([NH:10][C:11]2[C:12]3[C:19]4[CH2:20][CH2:21][N:22]([C:31](=[O:32])/[CH:30]=[CH:29]/[CH2:28][N:27]([CH3:26])[CH:34]([CH3:36])[CH3:35])[CH2:23][C:18]=4[S:17][C:13]=3[N:14]=[CH:15][N:16]=2)=[CH:5][C:4]=1[OH:24]

参加物

6

反応物 4

HCID 81531DiisopropylethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 668498872,3-Dichloro-5-(5,6,7,8-tetrahydropyrido[4',3':4,5]thieno[2,3-d]pyrimidin-4-ylamino)phenol hydrochlorideHCID 86650197(2E)-4-[methyl(1-methylethyl)amino]but-2-enoic acid hydrochloride

生成物 1

HCID 58116988HCID 58116988、化合物収率 52%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

2,3-Dichloro-5-(5,6,7,8-tetrahydropyrido[4′,3′:4,5]thieno[2,3-d]pyrimidin-4-ylamino)phenol hydrochloride from Example 69A (51 mg, 0.13 mmol) and (2E)-4-[methyl(1-methylethyl)amino]but-2-enoic acid hydrochloride from Example 2A (34 mg, 0.18 mmol) were dissolved in DMF (1.5 mL), and DIPEA (82 mg, 0.63 mmol) and TBTU (61 mg, 0.19 mmol) were added. The mixture was stirred at rt overnight. The product was then directly isolated by preparative HPLC to yield 33 mg (52%) of the title compound.

後処理

  1. customThe product was then directly isolated by preparative HPLC

出典と根拠

ORDレコード
ord-98645de9a8544ce6a55f6f788ac6ebd6
出典データセット
uspto-grants-2013_09
特許番号
US08524722B2

反応ノート

読み込み中…