HCID 67263692, 화합물 → HCID 67264544, 화합물

HRID 1040833노트

반응식

HRID 1040833 반응식
[N+:1]([C:4]1[CH:22]=[CH:21][C:7]2[CH2:8][CH2:9][N:10]([CH2:13][C@H:14]([O:19][CH3:20])[C:15]([F:18])([F:17])[F:16])[CH2:11][CH2:12][C:6]=2[CH:5]=1)([O-])=O>CO.[Pd]>[F:18][C:15]([F:16])([F:17])[C@@H:14]([O:19][CH3:20])[CH2:13][N:10]1[CH2:11][CH2:12][C:6]2[CH:5]=[C:4]([NH2:1])[CH:22]=[CH:21][C:7]=2[CH2:8][CH2:9]1

참가 물질

4

반응물 1

HCID 67263692HCID 67263692, 화합물

생성물 1

HCID 67264544HCID 67264544, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

7-Nitro-3-((S)-3,3,3-trifluoro-2-methoxy-propyl)-2,3,4,5-tetrahydro-1H-benzo[d]azepine (171 mg, 0.538 mmol, 1.0 eq) was placed in methanol (20 mL) and 10% palladium on carbon (17 mg) was added. The reaction was hydrogenated at 25 psi for 30 minutes. The mixture was then filtered through celite and concentrated under reduced pressure to obtain 3-((S)-3,3,3-trifluoro-2-methoxy-propyl)-2,3,4,5-tetrahydro-1H-benzo[d]azepin-7-ylamine as a green amorphous solid (113 mg, 73%). LCMS (m/e) 289 (M+1); 1H-NMR (CDCl3, 400 MHz) δ 6.89 (d, 1H, J=7.5 Hz), 6.51-6.45 (m, 2H), 3.76-3.66 (m, 1H), 3.61 (s, 3H), 3.63-3.52 (m, 2H), 2.88-2.79 (m, 6H), 2.78-2.69 (m, 4H).

후처리

  1. filtrationThe mixture was then filtered through celite and
  2. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-e5a511e8fcb1476a99c429f4a5f3b033
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08552186B2

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