Triethylamine → 3,4-Difluoro-2-(2-fluoro-4-iodo-phenylamino)-N-(2-hydroxy-ethoxy)-5-(3-oxo-[1,4,2]dioxazinan-2-ylmethyl)-benzamide

HRID 2038641

反応式

HRID 2038641 の反応式
[F:1][C:2]1[C:3]([NH:22][C:23]2[CH:28]=[CH:27][C:26]([I:29])=[CH:25][C:24]=2[F:30])=[C:4]([CH:12]=[C:13]([CH2:16][NH:17][O:18][CH2:19][CH2:20][OH:21])[C:14]=1[F:15])[C:5]([NH:7][O:8][CH2:9][CH2:10][OH:11])=[O:6].C1C(=O)N(OC(ON2C(=O)CCC2=O)=O)[C:33](=[O:34])C1.CCN(CC)CC>C(Cl)Cl.C1COCC1>[F:1][C:2]1[C:3]([NH:22][C:23]2[CH:28]=[CH:27][C:26]([I:29])=[CH:25][C:24]=2[F:30])=[C:4]([CH:12]=[C:13]([CH2:16][N:17]2[C:33](=[O:34])[O:21][CH2:20][CH2:19][O:18]2)[C:14]=1[F:15])[C:5]([NH:7][O:8][CH2:9][CH2:10][OH:11])=[O:6]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 676246Di(succinimido) carbonateHCID 115774573,4-difluoro-2-(2-fluoro-4-iodo-phenylamino)-N-(2-hydroxy-ethoxy)-5-[(2-hydroxy-ethoxyamino)-methyl]-benzamide

生成物 1

HCID 116138803,4-Difluoro-2-(2-fluoro-4-iodo-phenylamino)-N-(2-hydroxy-ethoxy)-5-(3-oxo-[1,4,2]dioxazinan-2-ylmethyl)-benzamide収率 11.9%

試薬・触媒・溶媒 1

HCID 21919333Tetrahydrofurane dichloromethane溶媒

実験手順

3,4-Difluoro-2-(2-fluoro-4-iodo-phenylamino)-N-(2-hydroxy-ethoxy)-5-[(2-hydroxy-ethoxyamino)-methyl]-benzamide (100 mg, 0.185 mmol) obtained in Example 6, N,N′-disuccinimidyl carbonate (59 mg, 0.231 mmol) and NEt3 (113 mg, 1.12 mmol) were stirred in a mixed solvent of CH2Cl2/THF (1 mL/1 mL) at room temperature for 10 hours. The reaction mixture was purified by silica gel column chromatography (CH2Cl2/MeOH as a developing solvent) to give the title compound (12.5 mg).

後処理

  1. customThe reaction mixture was purified by silica gel column chromatography (CH2Cl2/MeOH as a developing solvent)

出典と根拠

ORDレコード
ord-2d930e8499ad457183644647007bae26
出典データセット
uspto-grants-2013_11
特許番号
US08575391B2

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