Succinic Acid → 7-Chloro-6-{5-[2-(cyclopropylmethyl-amino)-thiazol-4-yl]-pyridin-2-ylthiomethyl}-2,3,4,5-tetrahydro-1H-benzo[d]azepine Succinate

HRID 1670581ノート

反応式

HRID 1670581 の反応式
[C:1]([OH:8])(=[O:7])[CH2:2][CH2:3][C:4]([OH:6])=[O:5].[Cl:9][C:10]1[CH:20]=[CH:19][C:13]2[CH2:14][CH2:15][NH:16][CH2:17][CH2:18][C:12]=2[C:11]=1[CH2:21][S:22][C:23]1[CH:28]=[CH:27][C:26]([C:29]2[N:30]=[C:31]([NH:34][CH2:35][CH:36]3[CH2:38][CH2:37]3)[S:32][CH:33]=2)=[CH:25][N:24]=1>CO>[C:1]([OH:8])(=[O:7])[CH2:2][CH2:3][C:4]([OH:6])=[O:5].[Cl:9][C:10]1[CH:20]=[CH:19][C:13]2[CH2:14][CH2:15][NH:16][CH2:17][CH2:18][C:12]=2[C:11]=1[CH2:21][S:22][C:23]1[CH:28]=[CH:27][C:26]([C:29]2[N:30]=[C:31]([NH:34][CH2:35][CH:36]3[CH2:38][CH2:37]3)[S:32][CH:33]=2)=[CH:25][N:24]=1

参加物

4

反応物 2

HCID 1110Succinic AcidHCID 598222797-chloro-6-{5-[2-(cyclopropylmethyl-amino)-thiazol-4-yl]-pyridin-2-ylthiomethyl}-2,3,4,5-tetrahydro-1H-benzo[d]azepine

生成物 1

HCID 866237127-Chloro-6-{5-[2-(cyclopropylmethyl-amino)-thiazol-4-yl]-pyridin-2-ylthiomethyl}-2,3,4,5-tetrahydro-1H-benzo[d]azepine Succinate収率 98%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Add succinic acid (0.073 g, 0.619 mmol) to a mixture of 7-chloro-6-{5-[2-(cyclopropylmethyl-amino)-thiazol-4-yl]-pyridin-2-ylthiomethyl}-2,3,4,5-tetrahydro-1H-benzo[d]azepine (0.282 g, 0.618 mmol) in methanol (5 mL) at room temperature. Concentrate the reaction mixture in vacuo. Combine the residue with MTBE (5 mL) and concentrate three times to afford a pale yellow foam. Dry under high vacuum at room temperature overnight to obtain the title compound (0.348 g, 98%) as a pale yellow foam. MS (ES+) m/z: 457.0 (M+H)+.

後処理

  1. concentrationConcentrate the reaction mixture in vacuo
  2. concentrationconcentrate three times
  3. customto afford a pale yellow foam
  4. customDry under high vacuum at room temperature overnight

出典と根拠

ORDレコード
ord-d2834045a951443e9802d7b490df2e56
出典データセット
uspto-grants-2011_08
特許番号
US07994163B2

反応ノート

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