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3-Hydroxypyridine → HCID 71667762, 화합물

HRID 1056851
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HRID 1056851 반응식
[CH:1]1([N:4]([CH3:20])[C:5]2[C:6]3[C:15]4[CH2:16][CH2:17][CH2:18][CH2:19][C:14]=4[S:13][C:7]=3[N:8]=[C:9]([CH2:11][OH:12])[N:10]=2)[CH2:3][CH2:2]1.O[C:22]1[CH:23]=[N:24][CH:25]=[CH:26][CH:27]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.CC(OC(/N=N/C(OC(C)C)=O)=O)C>C1COCC1>[CH:1]1([N:4]([CH3:20])[C:5]2[C:6]3[C:15]4[CH2:16][CH2:17][CH2:18][CH2:19][C:14]=4[S:13][C:7]=3[N:8]=[C:9]([CH2:11][O:12][C:22]3[CH:23]=[N:24][CH:25]=[CH:26][CH:27]=3)[N:10]=2)[CH2:3][CH2:2]1
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참가 물질

6

반응물 4

HCID 79713-HydroxypyridineHCID 11776TriphenylphosphineHCID 5363146Diisopropyl azodicarboxylateHCID 71667761[4-(Cyclopropyl-methyl-amino)-5,6,7,8-tetrahydro-benzo[4,5]thieno[2,3-d]pyrimidin-2-yl]-methanol

생성물 1

HCID 71667762HCID 71667762, 화합물수율 11.1%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매
2회

실험 절차

To a mixture of [4-(cyclopropyl-methyl-amino)-5,6,7,8-tetrahydro-benzo[4,5]thieno[2,3-d]pyrimidin-2-yl]-methanol (0.25 g, 0.00086 mol), 3-hydroxypyridine (0.090 g, 0.00095 mol) & triphenylphosphine (0.24 g, 0.00095 mol) in THF (20 ml) was added DIAD (0.19 g, 0.00095 mol) in THF (5 ml), and the mixture was stirred at room temperature for 12 h. The reaction mixture was concentrated and the resulting crude material was purified by preparative HPLC to give cyclopropyl-methyl-[2-(pyridine-3-yloxymethyl)-5,6,7,8-tetrahydro-benzo[4,5]thieno[2,3-d]pyrimidin-4-yl]-amine (35 mg, 11%) as a brown residue. 1H NMR (400 MHz, CDCl3): δ 0.35-0.42 (m, 2H), 0.62-0.68 (m, 2H), 1.72-1.78 (m, 2H), 1.88-1.97 (m, 2H), 2.80-2.90 (m, 5H), 3.00 (s, 3H), 5.24 (s, 2H), 7.16 (dd, 1H), 7.30 (dd, 1H), 8.17 (dd, 1H), 8.42 (d, 1H); LC-MS: [M+H]=367.3 m/z.

후처리

  1. concentrationThe reaction mixture was concentrated
  2. customthe resulting crude material was purified by preparative HPLC

출처 및 근거

ORD 기록
ord-8dee65db858444c7a55fd4383e3cfc18
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09399647B2

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