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Pyrrolidine → HCID 22641468、化合物

HRID 2415486
ノート
印刷プレビュー

反応式

HRID 2415486 の反応式
[Cl:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:12][CH3:13])=[CH:9][CH:10]=2)[N:5]=[C:4]([NH2:14])[CH:3]=1.[NH:15]1[CH2:19][CH2:18][CH2:17][CH2:16]1>C(O)(C)C>[ClH:1].[CH3:13][O:12][C:8]1[CH:7]=[C:6]2[C:11]([C:2]([N:15]3[CH2:19][CH2:18][CH2:17][CH2:16]3)=[CH:3][C:4]([NH2:14])=[N:5]2)=[CH:10][CH:9]=1
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

4

反応物 2

HCID 31268PyrrolidineHCID 14067409HCID 14067409、化合物

生成物 1

HCID 22641468HCID 22641468、化合物収率 21%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

反応条件

温度
60 °C

実験手順

A solution of 319 mg (0.92 mmol) of 4-chloro-7-methoxy-quinolin-2-ylamine in 20 ml of isopropanol was treated with 130 mg (1.83 mmol) of pyrrolidine and heated at 60° C. for 6 h. The reaction mixture was cooled to RT, concentrated in vacuo. The residue was applied to a silica gel column with hexane/AcOEt (1:1) as eluent. The purified fractions were combined and concentrated in vacuo upon which the desired product crystallized out. The crystals were filtered off and dried in a high vacuum to give 48 mg (21%) of 7-methoxy-4-pyrrolidin-1-yl-quinolin-2-ylamine hydrochloride as a light brown solid. EI mass spectrum, m/e: 243.2 (M calculated for C14H17N3O: 243).

後処理

  1. temperatureThe reaction mixture was cooled to RT
  2. concentrationconcentrated in vacuo
  3. concentrationconcentrated in vacuo upon which the desired product
  4. customcrystallized out
  5. filtrationThe crystals were filtered off
  6. customdried in a high vacuum

出典と根拠

ORDレコード
ord-318690c4ed104725b68a60b5535f62f2
出典データセット
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06818767B2

反応ノート

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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