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4-Methylmorpholine → HCID 18661240、化合物

HRID 849717
ノート
印刷プレビュー

反応式

HRID 849717 の反応式
CN1CCOCC1.Cl.[NH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][OH:17].[C:18]([O:22][C:23]([NH:25][C@H:26]([C:37](O)=[O:38])[CH2:27][C:28]1[C:36]2[C:31](=[CH:32][CH:33]=[CH:34][CH:35]=2)[NH:30][CH:29]=1)=[O:24])([CH3:21])([CH3:20])[CH3:19].ON1C2C=CC=CC=2N=N1.CCN=C=NCCCN(C)C.Cl>CN(C=O)C>[OH:17][CH2:16][CH2:15][CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][NH:9][C:37](=[O:38])[C@H:26]([CH2:27][C:28]1[C:36]2[C:31](=[CH:32][CH:33]=[CH:34][CH:35]=2)[NH:30][CH:29]=1)[NH:25][C:23]([O:22][C:18]([CH3:21])([CH3:19])[CH3:20])=[O:24]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 79724-MethylmorpholineHCID 757711-HydroxybenzotriazoleHCID 83169N-tert-Butoxycarbonyl-L-tryptophanHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 193675137-Aminoheptan-1-ol hydrochloride

生成物 1

HCID 18661240HCID 18661240、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

N-Methylmorpholine (2.2 mL, 19.7 mmol) was added dropwise at room temperature to 7-amino-1-heptanol hydrochloride salt (3.3 g, 19.7 mmol), in 50 mL of dry DMF under argon with stirring. After stirring for 5 minutes the following were added: N-t-butoxycarbonyl-L-tryptophan, (5 g, 16.45 mmol), 1-hydroxybenzotriazole, (2.52 g, 16.45 mmol) and EDCI hydrochloride (4.73 g, 24.7 mmol). The mixture was stirred for 2 hours and then the DMF removed under reduced pressure. The residue was taken up in cold 2.5% HCl (100 mL) and ethyl acetate (3×100 mL) and transferred to a separatory funnel. The organic phase was isolated and washed consecutively with cold 2.5% HCl (100 mL) and then brine (100 mL). The ethyl acetate phase was dried (MgSO4), filtered and concentrated to obtain N-t-butoxycarbonyl-L-tryptophan-(7-hydroxyheptyl)amide; IR (neat): 3300, 2921, 1685, 1645, 1490, 1356, 1157 cm-1 ; 1H NMR (80 MHz, CDCl3): δ 0.98-1.62 (m, 10H, --(CH2)5 --), 1.45 (s, 9H, t-butyl), 2.86-3.32 (m, 4H,CH--CH2, HN--CH2), 3.68 (t, 2H, J=5.6 Hz, --CH2OH), 4.22-4.55 (m, 1H, CH), 5.12-5.32 (broad d, 1H, NH--CH), 5.65-5.9 (broad t, 1H, NH--CH2), 6.98-7.92 (m, 5H, ArH), 8.63 (broad 8, indole NH).

後処理

  1. stirringAfter stirring for 5 minutes the
  2. additionfollowing were added
  3. stirringThe mixture was stirred for 2 hours
  4. customthe DMF removed under reduced pressure
  5. customtransferred to a separatory funnel
  6. customThe organic phase was isolated
  7. washwashed consecutively with cold 2.5% HCl (100 mL)
  8. dry with materialThe ethyl acetate phase was dried (MgSO4)
  9. filtrationfiltered
  10. concentrationconcentrated

出典と根拠

ORDレコード
ord-59c3e01fd0ad483ebf8606ce1c6fd9c1
出典データセット
uspto-grants-2000_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06013792

反応ノート

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