Triethylamine → HCID 57488841、化合物

HRID 2114352ノート

反応式

HRID 2114352 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][C:11]([CH:14]([N:22]([CH3:39])[C:23](=[O:38])[CH2:24][N:25]3[C:30]4[CH:31]=[C:32]([Cl:36])[C:33]([Cl:35])=[CH:34][C:29]=4[O:28][CH2:27][C:26]3=[O:37])[CH2:15][N:16]3[CH2:21][CH2:20][O:19][CH2:18][CH2:17]3)=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.[CH2:40]([S:42](Cl)(=[O:44])=[O:43])[CH3:41].C(N(CC)CC)C>ClCCl>[Cl:36][C:32]1[C:33]([Cl:35])=[CH:34][C:29]2[O:28][CH2:27][C:26](=[O:37])[N:25]([CH2:24][C:23]([N:22]([CH:14]([C:11]3[CH:12]=[CH:13][C:8]([C:5]4[CH:4]=[CH:3][C:2]([NH:1][S:42]([CH2:40][CH3:41])(=[O:44])=[O:43])=[CH:7][CH:6]=4)=[CH:9][CH:10]=3)[CH2:15][N:16]3[CH2:17][CH2:18][O:19][CH2:20][CH2:21]3)[CH3:39])=[O:38])[C:30]=2[CH:31]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 11667Ethanesulfonyl chlorideHCID 46846402N-[1-(4'-amino-4-biphenylyl)-2-(4-morpholinyl)ethyl]-2-(6,7-dichloro-3-oxo-2,3-dihydro-4H-1,4-benzoxazin-4-yl)-N-methylacetamide

生成物 1

HCID 57488841HCID 57488841、化合物収率 23.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of N-[1-(4′-amino-4-biphenylyl)-2-(4-morpholinyl)ethyl]-2-(6,7-dichloro-3-oxo-2,3-dihydro-4H-1,4-benzoxazin-4-yl)-N-methylacetamide (68 mg, 0.12 mmol) in dichloromethane (2 mL) was added ethanesulfonyl chloride (18.5 mg, 0.14 mmol). Triethylamine (24 mg, 0.24 mmol) was added, and the resultant mixture was stirred at room temperature for 2 h. The mixture was concentrated under reduced pressure, and the residue was purified by Gilson preparative HPLC (Xterra Prep RP, 30×100 mm, 45 mL/min, A: acetonitrile with 0.1% TFA B: water with 0.1% TFA, A: 25 to 55% over 15 min, UV detection at 214 nm) to give 18.3 mg (23%) of the title compound as an off white solid. MS (ES) m/e 661.1 [M+H]+.

後処理

  1. concentrationThe mixture was concentrated under reduced pressure
  2. customthe residue was purified by Gilson preparative HPLC (Xterra Prep RP, 30×100 mm, 45 mL/min

出典と根拠

ORDレコード
ord-cad787e82956442398b7215906d06b9a
出典データセット
uspto-grants-2008_10
特許番号
US07432258B2

反応ノート

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