Hydrochloric Acid → 6-carboxy-4-(3-chloroanilino)-7H-pyrrolo[2,3-d]pyrimidine

HRID 567756ノート

反応式

HRID 567756 の反応式
O[Li].[OH2:3].[Cl:4][C:5]1[CH:6]=[C:7]([CH:23]=[CH:24][CH:25]=1)[NH:8][C:9]1[C:10]2[CH:19]=[C:18](OCC)[NH:17][C:11]=2[NH:12][C:13](=C=O)[N:14]=1.Cl.[CH3:27][OH:28]>O>[C:27]([C:18]1[NH:17][C:11]2[N:12]=[CH:13][N:14]=[C:9]([NH:8][C:7]3[CH:23]=[CH:24][CH:25]=[C:5]([Cl:4])[CH:6]=3)[C:10]=2[CH:19]=1)([OH:28])=[O:3]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 168937Lithium hydroxide, monohydrateHCID 1765196754-(3-chloroanilino)-6-ethoxy-carbonyl-7H-pyrrolo[2,3-d]pyrimidine

生成物 1

HCID 212626746-carboxy-4-(3-chloroanilino)-7H-pyrrolo[2,3-d]pyrimidine

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of 25 mg (0.6 mmol) of LiOH.H2O in 0.4 ml of H2O is added dropwise to a suspension of 95 mg (0.30 mmol) of 4-(3-chloroanilino)-6-ethoxy-carbonyl-7H-pyrrolo[2,3-d]pyrimidine (see stage1.4) in 0.7 ml of methanol and the mixture is heated to boiling for 4.5 h. It is cooled in an ice bath and acidified with 0.6 ml of 1 normal HCl solution. Filtering off and washing with water yields 6-carboxy-4-(3-chloroanilino)-7H-pyrrolo[2,3-d]pyrimidine; HPLC: tRet(Grad20)=8.7; FAB-MS: (M+H)+=289.

後処理

  1. temperaturethe mixture is heated
  2. temperatureIt is cooled in an ice bath
  3. filtrationFiltering off
  4. washwashing with water

出典と根拠

ORDレコード
ord-b9143c73542147fba59832036551e43c
出典データセット
uspto-grants-2001_01
特許番号
US06180636B2

反応ノート

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