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Hydrochloric Acid → 3-Carbamoyl-7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-phthalide

HRID 22165
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HRID 22165 반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[N:6]=[C:5]([O:11][C:12]2[CH:13]=[CH:14][CH:15]=[C:16]3[C:21]=2[C:19](=[O:20])[O:18][CH:17]3O)[N:4]=1.[C-:23]#[N:24].[K+].Cl.[OH2:27]>>[C:23]([CH:17]1[C:16]2[C:21](=[C:12]([O:11][C:5]3[N:4]=[C:3]([O:2][CH3:1])[CH:8]=[C:7]([O:9][CH3:10])[N:6]=3)[CH:13]=[CH:14][CH:15]=2)[C:19](=[O:20])[O:18]1)(=[O:27])[NH2:24]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 9032Potassium CyanideHCID 199274177-[(4,6-Dimethoxy-pyrimidin-2-yl)oxy]-3-hydroxy-phthalide

생성물 1

HCID 199274243-Carbamoyl-7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-phthalide

실험 절차

1.0 g of 7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-3-hydroxy-phthalide (see Example 84) is introduced into a solution of 2.1 g of potassium cyanide in 15 ml of water and the whole is treated dropwise at from -7° to -3° C., with cooling, over a period of 10 minutes, with 10 ml of concentrated hydrochloric acid. It is subsequently stirred at room temperature for approximately 16 hours and the crystals which have separated are then filtered off. They are washed with water and recrystallised from acetone/n-hexane to yield 0.2 g of 3-carbamoyl-7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-phthalide (see also Example 17).

후처리

  1. additionthe whole is treated dropwise at from -7° to -3° C.
  2. customthe crystals which have separated
  3. filtrationare then filtered off
  4. washThey are washed with water
  5. customrecrystallised from acetone/n-hexane

출처 및 근거

ORD 기록
ord-5db9dc541d104704a857d69cebb76a01
출처 데이터셋
uspto-grants-1995_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05428002

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