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 1670581노트

반응식

HRID 1670581 반응식
[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

참가 물질

4

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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)+.

후처리

  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

출처 및 근거

ORD 기록
ord-d2834045a951443e9802d7b490df2e56
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07994163B2

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