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

HRID 567756노트

반응식

HRID 567756 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-b9143c73542147fba59832036551e43c
출처 데이터셋
uspto-grants-2001_01
특허 번호
US06180636B2

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