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Triethylamine → 8-amino-9-fluoro-3-methyl-10-[(3-cyclopropylaminomethyl)-1-pyrrolidinyl]-7-oxo-2,3-dihydro-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylic acid

HRID 620890
ノート
印刷プレビュー

反応式

HRID 620890 の反応式
[NH2:1][C:2]1[C:15]2[C:14](=[O:16])[C:13]([C:17]([OH:19])=[O:18])=[CH:12][N:7]3[CH:8]([CH3:11])[CH2:9][O:10][C:5]([C:6]=23)=[C:4](F)[C:3]=1[F:21].[CH:22]1([NH:25][CH2:26][CH:27]2[CH2:31][CH2:30]NC2)[CH2:24][CH2:23]1.[CH2:32]([N:34](CC)CC)C>CN(C)C=O>[NH2:1][C:2]1[C:15]2[C:14](=[O:16])[C:13]([C:17]([OH:19])=[O:18])=[CH:12][N:7]3[CH:8]([CH3:11])[CH2:9][O:10][C:5]([C:6]=23)=[C:4]([N:34]2[CH2:32][CH2:30][CH2:31][CH:27]2[CH2:26][NH:25][CH:22]2[CH2:23][CH2:24]2)[C:3]=1[F:21]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 13491801N-(Pyrrolidin-3-ylmethyl)cyclopropanamineHCID 143913498-amino-9,10-difluoro-3-methyl-7-oxo-2,3-dihydro-7H-pyrido [1,2,3-de][1,4]benzoxazine-6-carboxylic acid

生成物 1

HCID 679063138-amino-9-fluoro-3-methyl-10-[(3-cyclopropylaminomethyl)-1-pyrrolidinyl]-7-oxo-2,3-dihydro-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylic acid

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

反応条件

温度
100 °C

実験手順

A mixture of 2.96 g (10 mmole) of 8-amino-9,10-difluoro-3-methyl-7-oxo-2,3-dihydro-7H-pyrido [1,2,3-de][1,4]benzoxazine-6-carboxylic acid, 2.1 g (15 mmole) of N-cyclopropyl-3-pyrrolidinemethanamine, 3.03 g (30 mmole) of triethylamine and 100 ml of N,N-dimethylformamide as heated at 100° C. for four hours. The solvent is removed in vacuo and the residue triturated with water. The aqueous suspension is adjusted to pH 7.2 with 1.0 M hydrochloric acid. The solid is removed by filtration, washed with water, and dried in vacuo to give 8-amino-9-fluoro-3-methyl-10-[(3-cyclopropylaminomethyl)-1-pyrrolidinyl]-7-oxo-2,3-dihydro-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylic acid.

後処理

  1. customThe solvent is removed in vacuo
  2. customthe residue triturated with water
  3. customThe solid is removed by filtration
  4. washwashed with water
  5. customdried in vacuo

出典と根拠

ORDレコード
ord-02192b84240d44c98f15a873eaa47b49
出典データセット
uspto-grants-1989_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04822801

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート