Hydrochloric Acid → HCID 131728370, 화합물

HRID 1158774노트

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HRID 1158774 반응식
O=[C:2]1[CH2:7][O:6][C@H:5]([C:8]2[CH:13]=[C:12]([F:14])[C:11]([F:15])=[CH:10][C:9]=2[F:16])[C@@H:4]([NH:17]C(=O)OC(C)(C)C)[CH2:3]1.[F:25][C:26]([F:38])([F:37])[C:27]1[N:28]=[CH:29][C:30]2[CH2:36][CH2:35][NH:34][CH2:33][C:31]=2[N:32]=1.[B][B][B][B][B][B][B][B][B][B].[ClH:49]>CO>[ClH:49].[ClH:49].[F:38][C:26]([F:25])([F:37])[C:27]1[N:28]=[CH:29][C:30]2[CH2:36][CH2:35][N:34]([C@H:2]3[CH2:7][O:6][C@H:5]([C:8]4[CH:13]=[C:12]([F:14])[C:11]([F:15])=[CH:10][C:9]=4[F:16])[C@@H:4]([NH2:17])[CH2:3]3)[CH2:33][C:31]=2[N:32]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 184565172-(Trifluoromethyl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidineHCID 59627525HCID 59627525, 화합물HCID 178419135HCID 178419135, 화합물

생성물 1

HCID 131728370HCID 131728370, 화합물

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

To a solution of 45 mg (0.13 mmol) of tert-butyl [(2R,3S)-5-oxo-2-(2,4,5-trifluorophenyl) tetrahydro-2H-pyran-3-yl]carbamate and 27 mg (0.13 mmol) of 2-(trifluoromethyl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidine in 2.0 mL of dry methanol was added 5.0 mg (0.039 mmol) of decaborane. The reaction mixture was stirred overnight and concentrated in vacuo, then purified by preparative thin layer chromatography using an Analtech® 1000 micron plate (5% methanol/methylene chloride, 1% concentrated ammonium hydroxide) to give the product which was stirred with hydrochloric acid in methanol (1.3M, 4 mL) for 1 h to give the title product. LC/MS 432.93 (M+1).

후처리

  1. concentrationconcentrated in vacuo
  2. custompurified by preparative thin layer chromatography
  3. customto give the product which

출처 및 근거

ORD 기록
ord-fe80365fd65d43319061378d365f4c72
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07812027B2

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