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(3aR,6aS)-2-methyl-octahydropyrrolo[3,4-c]pyrrole → 2-(2-Chloro-4-(1-methyl-1H-pyrazol-4-yl)phenyl)-5-((3aR,6aS)-5-methylhexahydropyrrolo[3,4-c]pyrrol-2(1H)-yl)-1,3,4-thiadiazole

HRID 579348
ノート
印刷プレビュー

反応式

HRID 579348 の反応式
Br[C:2]1[S:3][C:4]([C:7]2[CH:12]=[CH:11][C:10]([C:13]3[CH:14]=[N:15][N:16]([CH3:18])[CH:17]=3)=[CH:9][C:8]=2[Cl:19])=[N:5][N:6]=1.[CH3:20][N:21]1[CH2:28][C@@H:27]2[C@@H:23]([CH2:24][NH:25][CH2:26]2)[CH2:22]1>CN1C(=O)CCC1.C(Cl)Cl>[Cl:19][C:8]1[CH:9]=[C:10]([C:13]2[CH:14]=[N:15][N:16]([CH3:18])[CH:17]=2)[CH:11]=[CH:12][C:7]=1[C:4]1[S:3][C:2]([N:25]2[CH2:26][C@@H:27]3[C@@H:23]([CH2:22][N:21]([CH3:20])[CH2:28]3)[CH2:24]2)=[N:6][N:5]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 12958532(3aR,6aS)-2-methyl-octahydropyrrolo[3,4-c]pyrroleHCID 902824152-bromo-5-(2-chloro-4-(1-methyl-1H-pyrazol-4-yl)phenyl)-1,3,4-thiadiazole

生成物 1

HCID 902823752-(2-Chloro-4-(1-methyl-1H-pyrazol-4-yl)phenyl)-5-((3aR,6aS)-5-methylhexahydropyrrolo[3,4-c]pyrrol-2(1H)-yl)-1,3,4-thiadiazole収率 13%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒
HCID 13387
N-methyl-2-pyrrolidone
溶媒

反応条件

温度
120 °C

実験手順

A stirred suspension of 2-bromo-5-(2-chloro-4-(1-methyl-1H-pyrazol-4-yl)phenyl)-1,3,4-thiadiazole (70 mg, 0.197 mmol) and (3aR,6aS)-2-methyloctahydropyrrolo[3,4-c]pyrrole (75 mg, 0.590 mmol) in NMP (0.5 mL) was heated to 120° C. and the resulting solution was stirred for 16 hours. The reaction mixture was diluted with DCM (20 mL) and washed with saturated NaHCO3(aq) (20 mL). The organic phase was separated and the aqueous phase was re-extracted with DCM (20 mL). The combined organic phases were concentrated in vacuo to afford the crude product as a dark brown oily residue. The crude material was purified by mass directed preparative HPLC under acidic conditions (TFA modified) and the product containing fractions were loaded onto a 1 g SCX cartridge (pre-wet with MeOH). The cartridge was washed with MeOH (15 mL) then flushed with 7M NH3 in MeOH (10 mL). The MeOH/NH3 was removed in vacuo to afford the title compound as a light brown solid (10 mg, 13% yield). LC-MS: Rt 0.79 min; MS m/z 401.4 [M+H]+ [Method D]. 1H NMR (400 MHz, DMSO-d6) δ ppm 8.32 (s, 1H), 7.99-8.03 (m, 2H), 7.84 (d, J=2.02 Hz, 1H), 7.65-7.69 (m, 1H), 3.88 (s, 3H), 3.70 (dd, J=10.61, 8.08 Hz, 2H), 3.36 (dd, J=10.61, 3.03 Hz, 2H), 2.99 (br. s., 2H), 2.55 (br. s., 4H), 2.25 (s, 3H). 1H NMR (400 MHz, CHLOROFORM-d) δ ppm 8.21 (d, J=8.08 Hz, 1H), 7.81 (s, 1H), 7.69 (s, 1H), 7.57 (d, J=2.02 Hz, 1H), 7.46 (dd, J=8.34, 1.77 Hz, 1H), 3.99 (s, 3H), 3.79 (dd, J=9.85, 7.83 Hz, 2H), 3.53 (d, J=11.12 Hz, 2H), 3.12 (br. s., 2H), 2.76 (br. s., 2H), 2.58 (d, J=8.08 Hz, 2H), 2.41 (br. s., 3H).

後処理

  1. washwashed with saturated NaHCO3(aq) (20 mL)
  2. customThe organic phase was separated
  3. extractionthe aqueous phase was re-extracted with DCM (20 mL)
  4. concentrationThe combined organic phases were concentrated in vacuo
  5. customto afford the crude product as a dark brown oily residue
  6. customThe crude material was purified by mass
  7. additionthe product containing fractions
  8. washThe cartridge was washed with MeOH (15 mL)
  9. customthen flushed with 7M NH3 in MeOH (10 mL)
  10. customThe MeOH/NH3 was removed in vacuo

出典と根拠

ORDレコード
ord-5b0ec25004bd4a10849b70d8dd2a757b
出典データセット
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09040712B2

反応ノート

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