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Sodium triacetoxyborohydride → HCID 178521405、化合物

HRID 1051439
ノート
印刷プレビュー

反応式

HRID 1051439 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.[NH:24]1[CH:28]=[CH:27][C:26]([NH2:29])=[N:25]1.[BH-](OC(C)=O)(OC(C)=O)OC(C)=O.[Na+]>C(Cl)Cl>[NH:24]1[CH:28]=[CH:27][C:26]([NH:29][CH2:18][C:17]2[CH:16]=[C:15]([CH:22]=[CH:21][CH:20]=2)[O:14][CH2:13][CH:12]([OH:23])[CH2:11][N:2]2[CH2:3][CH2:4][C:5]3[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=3)[CH2:1]2)=[N:25]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 5049666Sodium triacetoxyborohydrideHCID 86729224HCID 86729224、化合物HCID 178418806HCID 178418806、化合物

生成物 1

HCID 178521405HCID 178521405、化合物収率 11%

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 1H-pyrazol-3-amine (80 mg, 0.96 mmol). The solution was heated at 60° C. for 0.5 h. NaBH(OAc)3 (204 mg, 0.96 mmol) was then added into the reaction mixture which was heated at 60° C. for another 1 h. The reaction mixture was quenched by adding 1 N HCl aqueous solution and diluted with DCM and washed with NaHCO3 aqueous solution. The separated organic layer was concentrated and the crude product was purified by preparative HPLC purification. (26 mg, yield 11%). MS (ESI+) e/z: 379.1 [M+1]. 1H NMR (MeOD, 400 MHz), δ ppm: 7.33-7.18 (m, 7H), 7.00-6.96 (m, 2H), 6.84-6.80 (m, 1H), 4.48-4.44 (m, 3H), 4.28 (s, 1H), 4.06-3.98 (m, 2H), 3.59-3.56 (m, 2H), 3.42-3.39 (m, 2H), 3.20-3.15 (m, 2H).

後処理

  1. temperaturewas heated 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. washwashed 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-0669af161a71418fb3147dc90face945
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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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート