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Hydrochloric Acid → rac-3-Amino-7,7,7-trifluoro-2-methylheptan-2-ol hydrochloride

HRID 1624114
ノート
印刷プレビュー

反応式

HRID 1624114 の反応式
C1CCCCC=1.[F:7][C:8]([F:29])([F:28])[CH2:9][CH2:10][CH2:11][CH:12]([NH:17]C(=O)OCC1C=CC=CC=1)[C:13]([OH:16])([CH3:15])[CH3:14].[ClH:30]>[Pd].C(O)C.C(OCC)C>[ClH:30].[NH2:17][CH:12]([CH2:11][CH2:10][CH2:9][C:8]([F:7])([F:28])[F:29])[C:13]([CH3:14])([OH:16])[CH3:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 313Hydrochloric AcidHCID 8079CyclohexeneHCID 86718190Rac-benzyl (7,7,7-trifluoro-2-hydroxy-2-methylheptan-3-yl)carbamate

生成物 1

HCID 86718188rac-3-Amino-7,7,7-trifluoro-2-methylheptan-2-ol hydrochloride

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 702Ethanol
溶媒
HCID 3283Diethyl Ether溶媒

実験手順

Under argon, 319 mg (0.30 mmol, 10% pure) of palladium on activated carbon and 9.1 ml (90.0 mmol) of cyclohexene were added to 1.0 g (3.0 mmol) of rac-benzyl (7,7,7-trifluoro-2-hydroxy-2-methylheptan-3-yl)carbamate Example 101A in ethanol (21 ml), and the reaction mixture was stirred at reflux overnight. The mixture was filtered through a Millipore® filter and the filter cake was washed with ethanol. 3 ml (6.0 mmol) of 2 N hydrochloric acid in diethyl ether were added to the filtrate and the mixture was concentrated and dried under high vacuum. This gave 785 mg (111% of theory) of the target compound. The product was used without further purification for the next reaction.

後処理

  1. temperatureat reflux overnight
  2. filtrationThe mixture was filtered through a Millipore®
  3. filtrationfilter
  4. washthe filter cake was washed with ethanol
  5. concentrationthe mixture was concentrated
  6. customdried under high vacuum
  7. customThe product was used without further purification for the next reaction

出典と根拠

ORDレコード
ord-5d57c30a5b954323ba4aa66d4e2b0456
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08778964B2

反応ノート

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