tert-Butyl piperazine-1-carboxylate → HCID 66868625、化合物

HRID 242092ノート

反応式

HRID 242092 の反応式
Br[C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[O:12][CH3:13])[CH:8]([C:14]1([C:18]3[CH:23]=[CH:22][C:21]([Cl:24])=[CH:20][CH:19]=3)[CH2:17][CH2:16][CH2:15]1)[NH:7][CH2:6][CH2:5]2.[C:25]([N:32]1[CH2:37][CH2:36][NH:35][CH2:34][CH2:33]1)([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26].C1(P(C2CCCCC2)C2C=CC=CC=2C2C(N(C)C)=CC=CC=2)CCCCC1>C1(C)C=CC=CC=1>[Cl:24][C:21]1[CH:20]=[CH:19][C:18]([C:14]2([CH:8]3[C:9]4[C:4](=[CH:3][C:2]([N:35]5[CH2:34][CH2:33][N:32]([C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])[CH2:37][CH2:36]5)=[C:11]([O:12][CH3:13])[CH:10]=4)[CH2:5][CH2:6][NH:7]3)[CH2:15][CH2:16][CH2:17]2)=[CH:23][CH:22]=1

参加物

5

反応物 3

HCID 143452tert-Butyl piperazine-1-carboxylateHCID 27342172-(Dicyclohexylphosphino)-2'-(dimethylamino)biphenylHCID 66869005HCID 66869005、化合物

生成物 1

HCID 66868625HCID 66868625、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A solution of 6-bromo-1-[1-(4-chlorophenyl)cyclobutyl]-7-methoxy-1,2,3,4-tetrahydroisoquinoline (203 mg, 0.5 mmol), Boc-piperazine (93 mg, 0.5 mmol), tris(benzylideaceton)dipalladium (18 mg, 0.02 mmol), sodium-tert-butylate (48 mg, 0.5 mmol) and 2′-(dicyclohexylphosphino)-N,N-dimethylbiphenyl-2-amine 815.7 mg, 0.04 mmol) under nitrogen in toluene (5 ml) was heated in the microwave to 120° C. for 10 minutes. The solvent was removed, the residue dissolved in methylenehloride and extracted with water. The methylenehloride was evaporated and the remaining solid purified by chromatography. Yield: 56 mg (0.1 mmol, 20%)

後処理

  1. customThe solvent was removed
  2. dissolutionthe residue dissolved in methylenehloride
  3. extractionextracted with water
  4. customThe methylenehloride was evaporated
  5. customthe remaining solid purified by chromatography

出典と根拠

ORDレコード
ord-37eaa0f0ac6c4a81aecc267fe8e02f82
出典データセット
uspto-grants-2014_02
特許番号
US08653100B2

反応ノート

読み込み中…