N-[(6-chloropyridin-3-yl)methyl]-2,2-difluoroethanamine → HCID 44232235、化合物

HRID 1044333

反応式

HRID 1044333 の反応式
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][NH:9][CH2:10][CH:11]([F:13])[F:12])=[CH:4][CH:3]=1.O[C:15]1[CH2:19][O:18][C:17](=[S:20])[CH:16]=1>C(O)(=O)C>[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][N:9]([CH2:10][CH:11]([F:13])[F:12])[C:15]2[CH2:19][O:18][C:17](=[S:20])[CH:16]=2)=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 44604123N-[(6-chloropyridin-3-yl)methyl]-2,2-difluoroethanamineHCID 136184246HCID 136184246、化合物

生成物 1

HCID 44232235HCID 44232235、化合物収率 29.1%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

105 mg (0.506 mmol) of N-[(6-chloropyridin-3-yl)methyl]-2,2-difluoroethanamine (which can be prepared according to: WO 2007/115644 A1, WO 2008/009360 A2) were added to 20 mg (0.169 mMol) of 4-hydroxyfuran-2(5H)-thione (known from: R. Labruère et al., Synthesis 4163-4166, 2006) in 0.5 ml of acetic acid, and the mixture was stirred at room temperature for 14 days. Concentration under reduced pressure and purification of the residue by preparative HPLC (RP18, CH3CN—H2O) gave 15 mg (yield: 28.8% of theory) of 4-{[(6-chloropyridin-3-yl)methyl](2,2-difluoroethyl)amino}furan-2(5H)-thione.

後処理

  1. concentrationConcentration
  2. customunder reduced pressure and purification of the residue by preparative HPLC (RP18, CH3CN—H2O)

出典と根拠

ORDレコード
ord-41b80943c48249bfbf32e485443092a3
出典データセット
uspto-grants-2013_10
特許番号
US08563584B2

関連ノート

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