Triphenylphosphine → HCID 68679430、化合物

HRID 2265877ノート

反応式

HRID 2265877 の反応式
[F:1][C:2]1[CH:32]=[CH:31][C:5]([O:6][C:7]2[CH:12]=[CH:11][C:10]([S:13]([N:16]3[CH2:25][CH2:24][C:23]4[C:18](=[CH:19][CH:20]=[C:21]([OH:26])[CH:22]=4)[CH:17]3[C:27]([O:29][CH3:30])=[O:28])(=[O:15])=[O:14])=[CH:9][CH:8]=2)=[CH:4][CH:3]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.CCOC(/N=N/C(OCC)=O)=O.[CH3:64][N:65]1[CH2:70][CH2:69][N:68]([CH2:71][CH2:72][CH2:73]O)[CH2:67][CH2:66]1>C1COCC1>[F:1][C:2]1[CH:3]=[CH:4][C:5]([O:6][C:7]2[CH:8]=[CH:9][C:10]([S:13]([N:16]3[CH2:25][CH2:24][C:23]4[C:18](=[CH:19][CH:20]=[C:21]([O:26][CH2:73][CH2:72][CH2:71][N:68]5[CH2:69][CH2:70][N:65]([CH3:64])[CH2:66][CH2:67]5)[CH:22]=4)[CH:17]3[C:27]([O:29][CH3:30])=[O:28])(=[O:14])=[O:15])=[CH:11][CH:12]=2)=[CH:31][CH:32]=1

参加物

6

反応物 4

HCID 11776TriphenylphosphineHCID 792083-(4-Methyl-1-piperazine)propan-1-olHCID 5462977Diethyl azodicarboxylateHCID 68679822Methyl 2-[4-(4-fluorophenoxy)benzenesulfonyl]-6-hydroxy-1,2,3,4-tetrahydro-isoquinoline-1-carboxylate

生成物 1

HCID 68679430HCID 68679430、化合物収率 76%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

250 mg (0.55 mmol) of methyl 2-[4-(4-fluorophenoxy)benzenesulfonyl]-6-hydroxy-1,2,3,4-tetrahydroisoquinoline-1-carboxlate are dissolved in 5 ml of THF. At room temperature, 216 mg (0.825 mmol) of triphenylphosphine, 142 μl (0.825 mmol) of DEAD and 120 mg (0.825 mmol) of 3-(4-methylpiperazin-1-yl)propan-1-ol are added, and the solution is stirred at room temperature for 18 hours. The solvent is then removed, and the residue is chromatographed on silica gel, allowing the desired product to be isolated as a colorless solid. Yield 76%.

後処理

  1. customThe solvent is then removed
  2. customthe residue is chromatographed on silica gel
  3. customto be isolated as a colorless solid

出典と根拠

ORDレコード
ord-e929eec59fae4e6f8affd41005073166
出典データセット
uspto-grants-2010_12
特許番号
US07858619B2

反応ノート

読み込み中…