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Triethylamine → HCID 10410368、化合物

HRID 1435880
ノート
印刷プレビュー

反応式

HRID 1435880 の反応式
Cl.[CH3:2][O:3][C:4]1[N:5]=[C:6]2[C:11](=[CH:12][CH:13]=1)[N:10]=[CH:9][CH:8]=[C:7]2[C:14]1[CH:15]=[CH:16][C:17]([CH2:20][CH2:21][NH2:22])=[N:18][CH:19]=1.C(N(CC)CC)C.[O:30]1[C:39]2[CH:38]=[C:37]([CH:40]=O)[N:36]=[CH:35][C:34]=2[O:33][CH2:32][CH2:31]1.[BH4-].[Na+]>C(Cl)Cl.CCO>[O:30]1[C:39]2[CH:38]=[C:37]([CH2:40][NH:22][CH2:21][CH2:20][C:17]3[CH:16]=[CH:15][C:14]([C:7]4[C:6]5[C:11](=[CH:12][CH:13]=[C:4]([O:3][CH3:2])[N:5]=5)[N:10]=[CH:9][CH:8]=4)=[CH:19][N:18]=3)[N:36]=[CH:35][C:34]=2[O:33][CH2:32][CH2:31]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8471TriethylamineHCID 4311764Sodium borohydrideHCID 218736682,3-Dihydro[1,4]dioxino[2,3-c]pyridine-7-carbaldehydeHCID 68441439(2-{5-[6-(Methyloxy)-1,5-naphthyridin-4-yl]-2-pyridinyl}ethyl)amine hydrochloride salt

生成物 1

HCID 10410368HCID 10410368、化合物収率 168.7%

試薬・触媒・溶媒 2

HCID 702
Ethanol
溶媒
2 回
HCID 6344Dichloromethane溶媒

実験手順

To a stirred solution of (2-{5-[6-(methyloxy)-1,5-naphthyridin-4-yl]-2-pyridinyl}ethyl)amine hydrochloride salt (0.69 mmole) in dry CH2Cl2 (25 mL) and dry EtOH (10 mL) at RT was added triethylamine (0.29 mL, 2.07 mmole) and 2,3-dihydro[1,4]dioxino[2,3-c]pyridine-7-carbaldehyde (0.12 g, 0.73 mmole). After 24 h, the reaction contents were concentrated and dried under high vacuum. To a stirred solution of the crude imine in dry EtOH (25 mL) at RT was added NaBH4 (0.03 g, 0.73 mmole). After 24 h, Silica gel (5 g) was added to the reaction solution and the suspension was concentrated under vacuum to a dry solid. Purification on silica (CHCl3/MeOH, 9:1 containing 5% NH4OH) afforded the title compound (0.50 g, 72%) as light yellow solid: 1H NMR (400 MHz, CD3OD) δ 9.52 (d, J=1.8 Hz, 1H), 9.22 (d, J=5.6 Hz, 1H), 9.02 (d, J=8.3 Hz; 1H), 8.57 (m, 2H), 8.48 (d, J=5.6 Hz, 1H), 8.19 (d, J=9.3 Hz, 1H), 7.79 (s, 1H), 7.68 (d, J=9.3 Hz, 1H), 4.66 (m, 4H), 4.54 (s, 2H), 4.13 (s, 3H), 3.82 (m, 2H), 3.71 (s, 2H). LC-MS (ES) m/e 430 (M+H)+.

後処理

  1. customthe reaction contents
  2. concentrationwere concentrated
  3. customdried under high vacuum
  4. waitAfter 24 h
  5. additionSilica gel (5 g) was added to the reaction solution
  6. concentrationthe suspension was concentrated under vacuum to a dry solid
  7. customPurification on silica (CHCl3/MeOH, 9:1 containing 5% NH4OH)

出典と根拠

ORDレコード
ord-d71b24495a334c9e82d2e4bb0c87e561
出典データセット
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07618959B2

反応ノート

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