HCID 86731691, 화합물 → TERT-BUTYL (3-AMINO-1,1,1-TRIFLUOROPROPAN-2-YL)CARBAMATE

HRID 1504808노트

반응식

HRID 1504808 반응식
[F:1][C:2]([F:25])([F:24])[CH:3]([NH:16][C:17](=[O:23])[O:18][C:19]([CH3:22])([CH3:21])[CH3:20])[CH2:4][NH:5]C(=O)OCC1C=CC=CC=1>[Pd].CO>[NH2:5][CH2:4][CH:3]([NH:16][C:17](=[O:23])[O:18][C:19]([CH3:21])([CH3:20])[CH3:22])[C:2]([F:25])([F:1])[F:24]

참가 물질

4

반응물 1

HCID 86731691HCID 86731691, 화합물

생성물 1

HCID 84726007TERT-BUTYL (3-AMINO-1,1,1-TRIFLUOROPROPAN-2-YL)CARBAMATE

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

A mixture of benzyl tert-butyl (3,3,3-trifluoropropane-1,2-diyl)biscarbamate (160 g, 442 mmol) and palladium on carbon (10% w/w, 12 g) in methanol (1500 mL) was stirred at room temperature under a hydrogen atmosphere. After 16 hours, the reaction mixture was filtered. The filtrate was concentrated under reduced pressure, washed with hexane (500 mL), and dried in an oven under reduced pressure to afford tert-butyl (3-amino-1,1,1-trifluoropropan-2-yl)carbamate. MS ESI calc'd. for C8H16F3N2O2 [M+H]+ 229. found 229. 1H NMR (400 MHz, CDCl3) δ 5.30 (d, J=6.8 Hz, 1H), 4.23 (s, 1H), 3.10-2.98 (m, 2H), 1.63 (s, 2H), 1.46 (s, 9H).

후처리

  1. filtrationthe reaction mixture was filtered
  2. concentrationThe filtrate was concentrated under reduced pressure
  3. washwashed with hexane (500 mL)
  4. customdried in an oven under reduced pressure

출처 및 근거

ORD 기록
ord-bffddbd0c8044cbbbbff0b9d2e99d69f
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09216173B2

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