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Acetic Acid → (1S,2R)-2-(3-chlorophenyl)-1-(4-chlorophenyl)-N-(dicyclopropylmethyl)but-3-en-1-amine

HRID 932033
ノート
印刷プレビュー

反応式

HRID 932033 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C@@H:8]([CH:18]=[CH2:19])[C@@H:9]([C:11]2[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][CH:12]=2)[NH2:10])[CH:5]=[CH:6][CH:7]=1.[CH:20]1([C:23]([CH:25]2[CH2:27][CH2:26]2)=O)[CH2:22][CH2:21]1.C(O)(=O)C.C([BH3-])#N.[Na+]>CO.C(OCC)(=O)C>[Cl:1][C:2]1[CH:3]=[C:4]([C@@H:8]([CH:18]=[CH2:19])[C@@H:9]([C:11]2[CH:12]=[CH:13][C:14]([Cl:17])=[CH:15][CH:16]=2)[NH:10][CH:23]([CH:25]2[CH2:27][CH2:26]2)[CH:20]2[CH2:22][CH2:21]2)[CH:5]=[CH:6][CH:7]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 176Acetic Acid2 回HCID 70721Dicyclopropyl ketoneHCID 5003444Sodium cyanoborohydride2 回HCID 58573105(1S,2R)-2-(3-chlorophenyl)-1-(4-chlorophenyl)but-3-en-1-amine

生成物 1

HCID 67999637(1S,2R)-2-(3-chlorophenyl)-1-(4-chlorophenyl)-N-(dicyclopropylmethyl)but-3-en-1-amine

試薬・触媒・溶媒 2

HCID 887
Methanol
溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
50 °C

実験手順

To a solution of 2.0 g (6.84 mmol) of (1S,2R)-2-(3-chlorophenyl)-1-(4-chlorophenyl)but-3-en-1-amine (Example 115, Step E), dicyclopropyl ketone (7.54 mL, 68.4 mmol), and acetic acid (1.96 mL, 34.2 mmol) in methanol (25.0 mL) was added sodium cyanoborohydride (1.44 mL, 27.4 mmol) at rt. The resulting mixture was stirred at 50° C. for 2 days. Acetic acid (1.5 ml) and sodium cyanoborohydride (0.6 g) were added again and heating was continued overnight. 200 ml of ethyl acetate was added, and the organic layer was washed consecutively with K2CO3 solution and sat. NaCl solution, dried over K2CO3, filtered and the filtrate was concentrated under reduced pressure at 60° C. The mixture was purified by flash chromatography on silica gel (eluent: DCM/MeOH, 95/5) to give the title compound.

後処理

  1. temperatureheating
  2. waitwas continued overnight
  3. washthe organic layer was washed consecutively with K2CO3 solution and sat. NaCl solution
  4. dry with materialdried over K2CO3
  5. filtrationfiltered
  6. concentrationthe filtrate was concentrated under reduced pressure at 60° C
  7. customThe mixture was purified by flash chromatography on silica gel (eluent: DCM/MeOH, 95/5)

出典と根拠

ORDレコード
ord-ee362d582942414d99f61cb8e7683373
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09296736B2

反応ノート

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