Hydrochloric Acid → HCID 178487959, 화합물

HRID 1358569노트

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HRID 1358569 반응식
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[N:10]=[C:9]([CH2:11][O:12][C:13]3[CH:18]=[CH:17][C:16]([CH2:19][CH:20]([CH3:26])[C:21]([O:23]CC)=[S:22])=[CH:15][CH:14]=3)[N:8]([CH3:27])[C:7]=2[CH:28]=1.O.[OH-].[K+].[OH-].[K+].[ClH:34]>O1CCCC1.CN(C)C=O.O>[ClH:34].[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[N:10]=[C:9]([CH2:11][O:12][C:13]3[CH:18]=[CH:17][C:16]([CH2:19][CH:20]([CH3:26])[C:21]([OH:23])=[S:22])=[CH:15][CH:14]=3)[N:8]([CH3:27])[C:7]=2[CH:28]=1

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 14797Potassium Hydroxide2회HCID 23719240Potassium hydroxide monohydrateHCID 86587626HCID 86587626, 화합물

생성물 1

HCID 178487959HCID 178487959, 화합물

시약·촉매·용매 3

HCID 962Water용매2회HCID 6228Dimethylformamide용매3회HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of ethyl 3-[4-(6-methoxy-1-methyl-1H-benzimidazol-2-ylmethoxy)phenyl]-2-methylthiopropionate (2.0 g) in tetrahydrofuran (25 ml) were added successively potassium hydroxide monohydrate (0.42g), and dimethylformamide (5 ml). The mixture was stirred at room temperature for 2 hours. After addition of potassium hydroxide (0.42 g) and water (5 ml) the mixture was stirred at room temperature for 20 minutes. And then after addition of dimethylformamide (5 ml) the mixture was further stirred at room temperature for 1 hour and allowed to stand over night. To the reaction mixture was further added potassium hydroxide (0.42 g), water (5 ml) and dimethylformamide (5 ml) and the the mixture was stirred at 75° C. for 8 hours. The reaction mixture was poured into 1N hydrochloric acid (800 ml), stirred for 30 minutes and filtrated to give crystals. The crystals were washed successively with water, acetone and ethyl acetate and dried under reduced pressure to afford the title compound (1.27 g, mp 201-206° C.).

후처리

  1. stirringwas stirred at room temperature for 20 minutes
  2. stirringwas further stirred at room temperature for 1 hour
  3. waitto stand over night
  4. stirringthe the mixture was stirred at 75° C. for 8 hours
  5. stirringstirred for 30 minutes
  6. filtrationfiltrated
  7. customto give crystals
  8. washThe crystals were washed successively with water, acetone and ethyl acetate
  9. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-d70e37d1bd824422ba50bed35d6eaf8a
출처 데이터셋
uspto-grants-2003_07
특허 번호
US06596751B2

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