Hydrochloric Acid → 3-[5-(4-methyl-1,3-thiazol-2-yl)-2,4-dioxo-3,4-dihydro-1(2H)-pyrimidinyl]propanal

HRID 1925041노트

반응식

HRID 1925041 반응식
C[O:2][CH:3](OC)[CH2:4][CH2:5][N:6]1[CH:11]=[C:10]([C:12]2[S:13][CH:14]=[C:15]([CH3:17])[N:16]=2)[C:9](=[O:18])[NH:8][C:7]1=[O:19].Cl>O1CCCC1>[CH3:17][C:15]1[N:16]=[C:12]([C:10]2[C:9](=[O:18])[NH:8][C:7](=[O:19])[N:6]([CH2:5][CH2:4][CH:3]=[O:2])[CH:11]=2)[S:13][CH:14]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 594483511-[3,3-bis(methyloxy)propyl]-5-(4-methyl-1,3-thiazol-2-yl)-2,4(1H,3H)-pyrimidinedione

생성물 1

HCID 594483593-[5-(4-methyl-1,3-thiazol-2-yl)-2,4-dioxo-3,4-dihydro-1(2H)-pyrimidinyl]propanal

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a solution of 1-[3,3-bis(methyloxy)propyl]-5-(4-methyl-1,3-thiazol-2-yl)-2,4(1H,3H)-pyrimidinedione (Pre 44, 34 mg, 0.109 mmol) in Tetrahydrofuran (THF) (1.5 ml) 1M aqueous HCl (0.546 ml, 0.546 mmol) was added and the mixture was stirred at rt for 5 hrs. Other 1M aqueous HCl (0.273 ml, 0.273 mmol) was added and the mixture was stirred at rt overnight. Volatiles were evaporated (rotary, cold bath) and the residue was taken up with TEA (0.122 ml, 0.874 mmol) and THF (3 mL). The slurry was evaporated to dryness (rotary) to afford a crude that was used in the next reaction step assuming quantitative conversion to target compound (0.109 mmol) without any further purification

후처리

  1. stirringthe mixture was stirred at rt overnight
  2. customVolatiles were evaporated (rotary, cold bath)
  3. customThe slurry was evaporated to dryness (rotary)
  4. customto afford a crude that
  5. customwas used in the next reaction step
  6. customwithout any further purification

출처 및 근거

ORD 기록
ord-70ed00e04e6b4ef2baa98aec6a2de9c9
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08178549B2

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