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

HRID 1504808ノート

反応式

HRID 1504808 の反応式
[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]

参加物

4

反応物 1

HCID 86731691HCID 86731691、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-bffddbd0c8044cbbbbff0b9d2e99d69f
出典データセット
uspto-grants-2015_12
特許番号
US09216173B2

反応ノート

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