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Potassium Hydroxide → 2-[4-amino-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-7-yl]propionic acid

HRID 51500
ノート
印刷プレビュー

反応式

HRID 51500 の反応式
[NH2:1][C:2]1[C:3]2[C:10]([C:11]3[CH:16]=[CH:15][C:14]([O:17][C:18]4[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=4)=[CH:13][CH:12]=3)=[CH:9][N:8]([CH:24]([CH3:30])[C:25]([O:27]CC)=[O:26])[C:4]=2[N:5]=[CH:6][N:7]=1.[OH-].[K+]>CO>[NH2:1][C:2]1[C:3]2[C:10]([C:11]3[CH:16]=[CH:15][C:14]([O:17][C:18]4[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=4)=[CH:13][CH:12]=3)=[CH:9][N:8]([CH:24]([CH3:30])[C:25]([OH:27])=[O:26])[C:4]=2[N:5]=[CH:6][N:7]=1
参加物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 14797Potassium HydroxideHCID 22736339ethyl 2-[4-amino-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-7-yl]propionate

生成物 1

HCID 227363532-[4-amino-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-7-yl]propionic acid

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of ethyl 2-[4-amino-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-7-yl]propionate (201 mg), aqueous potassium hydroxide solution (4 ml of 2M solution) and methanol (20 ml) was boiled under reflux for 1 hour. The mixture was concentrated under reduced pressure to around 5 ml and then diluted with water (30 ml). The mixture was hot filtered and filtrate was cooled and then acidified with dilute acetic acid until no further precipitation occurred. The mixture was heated on a hot plate until the gel which had been obtained became a finely divided solid. The solid was collected by filtration to give 2-[4-amino-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-7-yl]propionic acid, m.p. 239.5-241° C.

後処理

  1. temperatureunder reflux for 1 hour
  2. concentrationThe mixture was concentrated under reduced pressure to around 5 ml
  3. additiondiluted with water (30 ml)
  4. filtrationThe mixture was hot filtered
  5. temperaturefiltrate was cooled
  6. customacidified with dilute acetic acid until no further precipitation
  7. temperatureThe mixture was heated on a hot plate until the gel which
  8. customhad been obtained
  9. filtrationThe solid was collected by filtration

出典と根拠

ORDレコード
ord-3e4ee56c3e2b413d9dc774cc6b0491a5
出典データセット
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06713474B2

反応ノート

読み込み中…

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