Hydrochloric Acid → HCID 67521251, 화합물

HRID 1926036노트

반응식

HRID 1926036 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([NH:17][C:18]2[C:19]3[NH:26][C:25]([CH2:27][NH:28]C(=O)OC(C)(C)C)=[CH:24][C:20]=3[N:21]=[CH:22][N:23]=2)[CH:5]=[CH:6][C:7]=1[O:8][CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([F:16])[CH:11]=1.[ClH:36].C(O)C>O1CCCC1>[ClH:1].[ClH:36].[NH2:28][CH2:27][C:25]1[NH:26][C:19]2[C:18]([NH:17][C:4]3[CH:5]=[CH:6][C:7]([O:8][CH2:9][C:10]4[CH:15]=[CH:14][CH:13]=[C:12]([F:16])[CH:11]=4)=[C:2]([Cl:1])[CH:3]=3)=[N:23][CH:22]=[N:21][C:20]=2[CH:24]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 702EthanolHCID 86626249Carbamic acid, N-[[4-[[3-chloro-4-[(3-fluorophenyl)methoxy]phenyl]amino]-5H-pyrrolo[3,2-d]pyrimidin-6-yl]methyl]-, 1,1-dimethylethyl ester

생성물 1

HCID 67521251HCID 67521251, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
60 °C

실험 절차

To a solution of tert-butyl [4-({3-chloro-4-[(3-fluorobenzyl)oxy]phenyl}amino)-5H-pyrrolo[3,2-d]pyrimidin-6-yl]methylcarbamate (500 mg) in tetrahydrofuran (12 mL) was added 2N hydrochloric acid (6.0 mL) at room temperature. The mixture was stirred at 60° C. for 2 hrs, ethanol was added to the reaction system and the mixture was concentrated under reduced pressure. The resultant crystals were collected by filtration and washed with diisopropyl ether to give the title compound (481.4 mg) as pale-yellow powder crystals.

후처리

  1. concentrationthe mixture was concentrated under reduced pressure
  2. filtrationThe resultant crystals were collected by filtration
  3. washwashed with diisopropyl ether

출처 및 근거

ORD 기록
ord-30aea98815ec4dfab332a9050ef94603
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08178543B2

반응 노트

불러오는 중…