3-Chloro-8-thia-4,6-diazatricyclo[7.4.0.0,2,7]trideca-1(9),2,4,6-tetraene → (5,6,7,8-Tetrahydro-benzo[4,5]thieno[2,3-d]pyrimidine-4-yl)-1,3-diaminopropane

HRID 1432186

反応式

HRID 1432186 の反応式
Cl[C:2]1[C:3]2[C:10]3[CH2:11][CH2:12][CH2:13][CH2:14][C:9]=3[S:8][C:4]=2[N:5]=[CH:6][N:7]=1>C(CN)CN.O>[N:5]1[C:4]2[S:8][C:9]3[CH2:14][CH2:13][CH2:12][CH2:11][C:10]=3[C:3]=2[C:2]([CH:2]([NH2:7])[CH2:3][CH2:4][NH2:5])=[N:7][CH:6]=1

参加物

4

反応物 1

HCID 6995153-Chloro-8-thia-4,6-diazatricyclo[7.4.0.0,2,7]trideca-1(9),2,4,6-tetraene

生成物 1

HCID 22182403(5,6,7,8-Tetrahydro-benzo[4,5]thieno[2,3-d]pyrimidine-4-yl)-1,3-diaminopropane収率 102.8%

試薬・触媒・溶媒 2

HCID 4281,3-Propanediamine溶媒HCID 962Water溶媒

実験手順

A solution of 4-chloro-5,6,7,8-tetrahydro-benzo[4,5]thieno[2,3-d]pyrimidine (0.5 g, 2.43 m. mol) in 1,3-diaminepropane (5 ml) was heated at 80° C. for 1 day. It was cooled to room temperature and then diluted with water (50 mL). The clear solution was cooled at 0° C. for overnight. The resulting solid was filtered and dried to get the title compound (0.3 g, 52%) as a brown color solid. 1H NMR (400 MHz, CD3OD): δ 8.20 (s, 1H), 3.65 (t, 2H), 2.95 (m, 2H), 2.80 (m, 4H), 1.80-2.00 (m, 6H). MS (ESI) m/z: Calculated: 262.37; Observed: 263.1 (M++1).

後処理

  1. temperatureThe clear solution was cooled at 0° C. for overnight
  2. filtrationThe resulting solid was filtered
  3. customdried

出典と根拠

ORDレコード
ord-72f7d97bf1b349699ea5e3ba66beba88
出典データセット
uspto-grants-2009_11
特許番号
US07612078B2

関連ノート

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