ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Acetic Acid → HCID 58958113、化合物

HRID 2252090
ノート
印刷プレビュー

反応式

HRID 2252090 の反応式
C[C:2]1[CH:11]=[C:10](N)[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.[CH3:13][C:14]1[CH:23]=[C:22]([NH:24][C:25]2[CH:26]=[C:27]([C:31]3[CH:36]=[CH:35][CH:34]=[C:33]([CH:37]=O)[CH:32]=3)[CH:28]=[CH:29][CH:30]=2)[C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[N:15]=1.[BH-](OC(C)=O)(OC(C)=O)OC(C)=O.[Na+].CC(O)=O>ClC(Cl)C>[CH2:4]1[C:9]2[C:10](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH2:11][CH2:2][N:3]1[CH2:37][C:33]1[CH:32]=[C:31]([C:27]2[CH:28]=[CH:29][CH:30]=[C:25]([NH:24][C:22]3[C:21]4[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=4)[N:15]=[C:14]([CH3:13])[CH:23]=3)[CH:26]=2)[CH:36]=[CH:35][CH:34]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 176Acetic AcidHCID 811164-Amino-2-methylquinolineHCID 5049666Sodium triacetoxyborohydrideHCID 58958219HCID 58958219、化合物

生成物 1

HCID 58958113HCID 58958113、化合物収率 55%

試薬・触媒・溶媒 1

HCID 63651,1-Dichloroethane
溶媒

実験手順

(3-Bromophenyl)-(2-methylquinolin-4-yl)amine (71). 71 is prepared from 70 by the procedure of Example 1 Step 3. Step 2. 3′-(2-Methylquinolin-4-ylamino)biphenyl-3-carbaldehyde (73). To a suspension of 71 (294 mg, 0.94 mmol) in toluene (9.6 mL) under N2 were sequentially added saturated NaHCO3 (aq. 3.8 mL), a solution of 72 (199 mg, 1.33 mmol) in EtOH (6.7 mL), and PdCl2(Ph3P)3 (32 mg, 0.046 mmol). The reaction was heated at 80° C. for 21 hours before it was allowed to cool to room temperature. The reaction mixture was extracted with ethyl acetate (40 mL) and washed with water (15 mL), brine (15 mL). The ethyl acetate extracts were dried over anhydrous magnesium sulfate and concentrated. The residue was chromatographed on silica gel (dichloromethane to 20:1 dichloromethane/methanol) to give 73 as a yellow solid (219 mg, 68.9%). Step 3.3′-(3,4-Dihydro-1H-isoquinolin-2-ylmethyl)biphenyl-3-yl]-(2-methylquinolin-4-yl)amine. To a solution of 73 (102 mg, 0.301 mmol) in dichloroethane (3.0 mL) under N2 was added 40 (0.04 mL, 0.315 mmol). The reaction was stirred for 24 minutes before the sequential addition of NaBH(OAc)3 (94 mg, 0.444 mmol) and AcOH (0.02 mL, 0.349 mmol). The reaction was stirred for 19 hours and then extracted with ethyl acetate (2×30 mL). The ethyl acetate extracts were washed with 2 N NaOH (aq. 15 mL), brine (15 mL), dried (MgSO4), and concentrated. The residue was chromatographed on silica gel (dichloromethane to 30:1 to 20:1dichloromethane/methanol) to give the desired product as a yellow solid (75 mg, 55%).

後処理

  1. extractionextracted with ethyl acetate (2×30 mL)
  2. washThe ethyl acetate extracts were washed with 2 N NaOH (aq. 15 mL), brine (15 mL)
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated
  5. customThe residue was chromatographed on silica gel (dichloromethane to 30:1 to 20:1dichloromethane/methanol)

出典と根拠

ORDレコード
ord-6a3c9f7a25ea4ed78ab35b67fbda0456
出典データセット
uspto-grants-2008_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07320989B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート