Hydroxyamine hydrochloride → 5-[3-[4-(4-Fluorophenyl)piperazin-1-yl]propyl]-4-hydroxyimino-2-methyl-2,3,4,5-tetrahydropyrrolo[2,3-e][1,2]thiazine 1,1-dioxide

HRID 2270442ノート

反応式

HRID 2270442 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][CH2:16][N:17]3[C:21]4[C:22](=O)[CH2:23][N:24]([CH3:28])[S:25](=[O:27])(=[O:26])[C:20]=4[CH:19]=[CH:18]3)[CH2:10][CH2:9]2)=[CH:4][CH:3]=1.Cl.[NH2:31][OH:32]>N1C=CC=CC=1>[F:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][CH2:16][N:17]3[C:21]4[C:22](=[N:31][OH:32])[CH2:23][N:24]([CH3:28])[S:25](=[O:27])(=[O:26])[C:20]=4[CH:19]=[CH:18]3)[CH2:10][CH2:9]2)=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 443297Hydroxyamine hydrochlorideHCID 99100415-[3-[4-(4-Fluorophenyl)piperazin-1-yl]propyl]-2-methyl-2,3,4,5-tetrahydropyrrolo[2,3-e][1,2]thiazin-4-one 1,1-dioxide

生成物 1

HCID 726120005-[3-[4-(4-Fluorophenyl)piperazin-1-yl]propyl]-4-hydroxyimino-2-methyl-2,3,4,5-tetrahydropyrrolo[2,3-e][1,2]thiazine 1,1-dioxide収率 83%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
60 °C

実験手順

A suspension of 168 mg (0.4 mmol) of Compound 25 and 111 mg (1.6 mmol) of hydroxylamine hydrochloride in 10 ml of pyridine was stirred for 21 hours over an oil bath of 60° C. Post-treatment was conducted in a similar manner as in Example 18. The residue was purified by chromatography on a silica gel column (eluent:methanol/chloroform=1/99), whereby 144 mg of the title compound were obtained (yield: 83%).

後処理

  1. customThe residue was purified by chromatography on a silica gel column (eluent:methanol/chloroform=1/99)

出典と根拠

ORDレコード
ord-cd190ca3a79748178c582e45200bddc5
出典データセット
uspto-grants-2001_12
特許番号
US06331623B1

反応ノート

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