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4-Aminotetrahydropyran → HCID 45227713、化合物

HRID 1051438
ノート
印刷プレビュー

反応式

HRID 1051438 の反応式
[CH2:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3][N:2]1[CH2:11][CH:12]([OH:23])[CH2:13][O:14][C:15]1[CH:16]=[C:17]([CH:20]=[CH:21][CH:22]=1)[CH:18]=O.[O:24]1[CH2:29][CH2:28][CH:27]([NH2:30])[CH2:26][CH2:25]1.[BH-](OC(C)=O)(OC(C)=O)OC(C)=O.[Na+]>C(Cl)Cl>[CH2:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3][N:2]1[CH2:11][CH:12]([OH:23])[CH2:13][O:14][C:15]1[CH:22]=[CH:21][CH:20]=[C:17]([CH2:18][NH:30][CH:27]2[CH2:28][CH2:29][O:24][CH2:25][CH2:26]2)[CH:16]=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

5

反応物 3

HCID 4192234-AminotetrahydropyranHCID 5049666Sodium triacetoxyborohydrideHCID 86729224HCID 86729224、化合物

生成物 1

HCID 45227713HCID 45227713、化合物収率 17%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
60 °C

実験手順

To a solution of 3-(3-(3,4-dihydroisoquinolin-2(1H)-yl)-2-hydroxypropoxy)benzaldehyde (200 mg, 0.64 mmol) in DCM (15 mL) was added tetrahydro-2H-pyran-4-amine (97 mg, 0.96 mmol). The solution was heated at 60° C. for 0.5 h. Then, NaBH(OAc)3 (204 mg, 0.96 mmol) was added into the reaction mixture and heated at 60° C. for another 1 h. The reaction mixture was quenched by adding 1 N HCl aqueous solution and diluted with DCM then washed with NaHCO3 aqueous solution. The separated organic layer was concentrated and the crude product was purified by preparative HPLC purification. (40 mg, yield 17%) MS (ESI+) e/z: 397.2 [M+1]+. 1H NMR (MeOD, 400 MHz), δ ppm: 7.36 (t, J=8.0 Hz, 1H), 7.19-7.15 (m, 3H), 7.11-7.02 (m, 4H), 4.39-4.33 (m, 1H), 4.16 (s, 2H), 4.08-4.00 (m, 6H), 3.49-3.40 (m, 3H), 3.25-3.20 (m, 2H), 3.15-3.03 (m, 4H), 2.12-2.02 (m, 2H), 1.71-1.60 (m, 2H).

後処理

  1. temperatureheated at 60° C. for another 1 h
  2. customThe reaction mixture was quenched
  3. additionby adding 1 N HCl aqueous solution
  4. additiondiluted with DCM
  5. washthen washed with NaHCO3 aqueous solution
  6. concentrationThe separated organic layer was concentrated
  7. customthe crude product was purified by preparative HPLC purification

出典と根拠

ORDレコード
ord-a3b4d908f81747fe9360e943d185fe5e
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09388173B2

反応ノート

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