Sodium Hydroxide → Sodium (4r)-4-methyl-4-(3-methylbutyl)-2-{7-[(1-naphthylsulfonyl)amino]-1,1-dioxido-4h-1,2,4-benzothiadiazin-3-yl}-3-oxo-3,4-dihydronaphthalen-1-olate

HRID 2224942ノート

反応式

HRID 2224942 の反応式
[OH:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C@@:5]([CH3:17])([CH2:12][CH2:13][CH:14]([CH3:16])[CH3:15])[C:4](=[O:18])[C:3]=1[C:19]1[NH:24][C:23]2[CH:25]=[CH:26][C:27]([NH:29][S:30]([C:33]3[C:42]4[C:37](=[CH:38][CH:39]=[CH:40][CH:41]=4)[CH:36]=[CH:35][CH:34]=3)(=[O:32])=[O:31])=[CH:28][C:22]=2[S:21](=[O:44])(=[O:43])[N:20]=1.[OH-].[Na+:46]>O>[CH3:17][C@@:5]1([CH2:12][CH2:13][CH:14]([CH3:16])[CH3:15])[C:6]2[C:11](=[CH:10][CH:9]=[CH:8][CH:7]=2)[C:2]([O-:1])=[C:3]([C:19]2[NH:24][C:23]3[CH:25]=[CH:26][C:27]([NH:29][S:30]([C:33]4[C:42]5[C:37](=[CH:38][CH:39]=[CH:40][CH:41]=5)[CH:36]=[CH:35][CH:34]=4)(=[O:32])=[O:31])=[CH:28][C:22]=3[S:21](=[O:44])(=[O:43])[N:20]=2)[C:4]1=[O:18].[Na+:46]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 136384722n-{3-[(4r)-1-Hydroxy-4-methyl-4-(3-methylbutyl)-3-oxo-3,4-dihydronaphthalen-2-yl]-1,1-dioxido-4h-1,2,4-benzothiadiazin-7-yl}naphthalene-1-sulfonamide

生成物 1

HCID 131726901Sodium (4r)-4-methyl-4-(3-methylbutyl)-2-{7-[(1-naphthylsulfonyl)amino]-1,1-dioxido-4h-1,2,4-benzothiadiazin-3-yl}-3-oxo-3,4-dihydronaphthalen-1-olate収率 68%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of Example 105A (30.0 mg, 0.048 mmol) and 0.998 M sodium hydroxide (0.048 mL, 0.048 mmol) in water (3 mL) was stirred at rt for 16 h. The reaction mixture was concentrated in vacuo to give the title compound (21 mg, 68% yield). 1H NMR (300 MHz, DMSO-d6) δ 0.40 m, 1 H) 0.65 (d, J=6.62 Hz, 3 H) 0.67 m, 3 H) 0.75 (m, 1 H) 1.26 (m, 1H) 1.34 (s, 3 H) 1.69 m, 1 H) 2.10 m, 1 H) 7.12 m, 2 H) 7.23 (s, 1 H) 7.29 (m, 1 H) 7.44 m, 2 H) 7.64 m, 2 H) 7.74 m, 1 H) 8.00 (d, J=7.72 Hz, 1 H) 8.07 (d, J=7.72 Hz, 1 H) 8.16 (d, J=7.35 Hz, 1 H) 8.20 m, 1 H) 8.76 (s, 1 H) 10.82 (s, 1 H) 15.39 (s, 1 H). MS (ESI+) m/z 652.0 (M+H)+, 630.0 (M+H—Na)+, 647 (M−Na+NH4)+, (ESI−) m/z 628.0 (M−H—Na)−.

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo

出典と根拠

ORDレコード
ord-16f412d21a9f4a84abdc4f189beec250
出典データセット
uspto-grants-2008_05
特許番号
US07378414B2

反応ノート

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