Hydrochloric Acid → HCID 19906372, 화합물

HRID 2371812노트

반응식

HRID 2371812 반응식
[BH4-].[Na+].[CH3:3][O:4][C:5]1[CH:6]=[C:7]([CH:12]=[CH:13][C:14]=1[CH2:15][CH:16]1[C:24]2[C:19](=[CH:20][CH:21]=[C:22]([NH:25]C(=O)C(F)(F)F)[CH:23]=2)[CH:18]=[CH:17]1)[C:8]([O:10][CH3:11])=[O:9].O1CCCC1.[ClH:37]>CO>[ClH:37].[NH2:25][C:22]1[CH:23]=[C:24]2[C:19]([CH2:18][CH:17]=[C:16]2[CH2:15][C:14]2[CH:13]=[CH:12][C:7]([C:8]([O:10][CH3:11])=[O:9])=[CH:6][C:5]=2[O:4][CH3:3])=[CH:20][CH:21]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 4311764Sodium borohydrideHCID 19906418HCID 19906418, 화합물

생성물 1

HCID 19906372HCID 19906372, 화합물수율 79%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Sodium borohydride (0.24 g), was added to a 0° C. mixture of methyl 3-methoxy-4-[6-(trifluoroacetamido)-1H-inden-1-ylmethyl]benzoate (1.25 g), tetrahydrofuran (14 ml) and methanol (2 ml). After 15 min, the reaction was stirred at room temperature for 2 h and cooled to 0° C. 1N Hydrochloric acid was added and the mixture was extracted with ethyl acetate. The organic layer was washed (sodium bicarbonate, water, brine) and dried (MgSO4). Evaporation, dissolution in ether (50 ml) and addition of ethereal hydrogen chloride (5 ml) afforded methyl 4-(6-amino-3H-inden-1-ylmethyl)-3-methyoxybenzoate hydrochloride (0.85 g, 79%) as a colorless solid; mp 213.0°-215.0° C.; MS(CI), m/e=310 (M+H).

후처리

  1. temperaturecooled to 0° C
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe organic layer was washed (sodium bicarbonate, water, brine)
  4. dry with materialdried (MgSO4)
  5. customEvaporation, dissolution in ether (50 ml)
  6. additionaddition of ethereal hydrogen chloride (5 ml)

출처 및 근거

ORD 기록
ord-717cd2045f71483f867ac967b10ed961
출처 데이터셋
uspto-grants-1992_03
특허 번호
US05095038

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