ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Acetic Acid → t-Butyl 4'-[[3(R)-[[3-amino-3-methyl-l-oxobutyl]amino]-2,3,4,5-tetrahydro-2-oxo-1H-1-benzazepin-1-yl]methyl][1,1'-biphenyl]-2-carboxylate acetate

HRID 1755791
ノート
印刷プレビュー

反応式

HRID 1755791 の反応式
C(OC([NH:11][C:12]([CH3:50])([CH3:49])[CH2:13][C:14]([NH:16][C@@H:17]1[CH2:23][CH2:22][C:21]2[CH:24]=[CH:25][CH:26]=[CH:27][C:20]=2[N:19]([CH2:28][C:29]2[CH:34]=[CH:33][C:32]([C:35]3[C:36]([C:41]([O:43][C:44]([CH3:47])([CH3:46])[CH3:45])=[O:42])=[CH:37][CH:38]=[CH:39][CH:40]=3)=[CH:31][CH:30]=2)[C:18]1=[O:48])=[O:15])=O)C1C=CC=CC=1.C(O)(=O)C>CO.[OH-].[Pd+2].[OH-]>[C:41]([OH:43])(=[O:42])[CH3:36].[NH2:11][C:12]([CH3:50])([CH3:49])[CH2:13][C:14]([NH:16][C@@H:17]1[CH2:23][CH2:22][C:21]2[CH:24]=[CH:25][CH:26]=[CH:27][C:20]=2[N:19]([CH2:28][C:29]2[CH:30]=[CH:31][C:32]([C:35]3[C:36]([C:41]([O:43][C:44]([CH3:46])([CH3:45])[CH3:47])=[O:42])=[CH:37][CH:38]=[CH:39][CH:40]=3)=[CH:33][CH:34]=2)[C:18]1=[O:48])=[O:15]
参加物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 176Acetic AcidHCID 228551634'-[[2,3,4,5-Tetrahydro-3(R)-[[3-methyl-1-oxo-3-[[(benzyloxy)carbonyl]amino] butyl]amino]-2-oxo-1H-1-benzazepin-1-yl]methyl]-[1,1'-biphenyl]-2-carboxylic acid 1,1-dimethylethyl ester

生成物 1

HCID 67788487t-Butyl 4'-[[3(R)-[[3-amino-3-methyl-l-oxobutyl]amino]-2,3,4,5-tetrahydro-2-oxo-1H-1-benzazepin-1-yl]methyl][1,1'-biphenyl]-2-carboxylate acetate収率 193.7%

試薬・触媒・溶媒 2

HCID 9942167
Palladium hydroxide
触媒
HCID 887Methanol溶媒

実験手順

To a solution of 400 mg (0.592 mmol) of t-butyl 4'-[[3(R)[[3-benzyloxycarbonylamino-3-methyl-1-oxobutyl]amino]-2,3,4,5-tetrahydro-2-oxo-1H-1-benzazepin-1-yl]methyl][1,1'-biphenyl]-2-carboxylate (prepared according to the procedure of Fisher et al, U.S. Pat. No. 5,206,235) in 10 mL of methanol was added 0.034 mL (0.59 mmol) of acetic acid and 80 mg (20% w/w) palladium hydroxide. The resulting mixture was stirred under a hydrogen atmosphere for 4 hours. Catalyst was removed by filtration through Celite and the solvent removed under vacuum to afford 345 mg (97%) of the product as a white solid. 1H NMR (400 MHz, CD3OD): δ1.17 (s, 9H), 1.37 (s, 3H), 1.41 (s, 3H), 1.92 (s, 3H), 2.17 (m, 1H), 2.35 (m, 1H), 2.45-2.75 (m, 4H), 4.41 (dd; 12, 8 Hz; 1H), 4.93 (d, 15 Hz, 1H), 5.37 (d, 16 Hz, 1H), 7.12-7.52 (m, 11H), 7.66 (d, 8 Hz, 1H). FAB-MS: calculated for C33H39N3O4 541; found 542 (M+H,100%).

後処理

  1. customCatalyst was removed by filtration through Celite
  2. customthe solvent removed under vacuum

出典と根拠

ORDレコード
ord-b3170d1a9ee44ca6ae5001a0d5e1a95a
出典データセット
uspto-grants-1995_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05438136

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート